微波辅助合成Ru(Ⅱ)配合物及其自组装多层膜

Microwave-Assisted Synthesis of Ru(Ⅱ) Complex and Self-Assembled Multilayer Film Formed by Alternating Layers of the Ru Complex

运用微波辅助合成技术制备得到对称性钌（Ⅱ）配合物,对该配合物进行了1H NMR,ESI-MS和TG分析。该钌配合物两端对称的磷酸基团可通过共价键作用组装到纳米铟锡金属氧化物导电玻璃（Indium Tin Oxides,ITO）表面,使ITO表面呈现亲水性。利用锆离子作为桥梁成功组装了钌多层膜,并对该多层膜进行了循环伏安法（Cyclic Voltammetry,CV）及紫外-可见吸收光谱法（Ultraviolet-visible absorption spectrometry,UV-Vis）等光电化学分析,实验结果表明层层自组装过程中膜沉积均匀,在0.53 V出现可逆的氧化还原峰,在300～600 nm的紫外可见区域出现强且宽的吸收峰,表明该钌配合物具有优良的光电性能。

A symmetrical ruthenium complex bearing phosphonic acid was prepared under the microwave irradiation and fully characterized by1 H NMR, ESI-MS and thermo gravimetric（TG） analysis. For the Ru complex, the phosphonic groups were selectively attached to the ITO through covalent interaction, resulting in the hydrophilic surface due to the appearance of the exposed other phosphonic-acid groups on the top. The Layer by layer（LBL） growth of molecular units was used to fabricate redox-active films of Ru complex, which was followed by the formation of Zr4＋-phosphonate layer. The buildup of the films was followed by monitoring cyclic voltammetry（CV） and ultraviolet-visible absorption spectrometry（UV-Vis） measurements. The results showed the electrode modified by multilayered film displayed reversible redox processes, and the Ru（Ⅱ/Ⅲ） oxidative peak was observed at ＋0.53 V. The plots of surface coverage versus number of layers show a linear relationship, which means a uniform layer structure is formed during the LBL process. UV-Vis spectra shows the prepared Ru film have strong absorptions between 300 nm and 600 nm. These findings show the Ru complex has good photoelectric properties.