Turner Elizabeth A, Rösner Harald, Fenske Dieter, Huang Yining, Corrigan John F
Department of Chemistry, The University of Western Ontario, London, Ontario N6A 5B7, Canada.
J Phys Chem B. 2006 Aug 24;110(33):16261-9. doi: 10.1021/jp060135c.
The binary materials ZnS, ZnSe, and ZnTe have been successfully prepared within the mesoporous framework of MCM-41 at room temperature through the use of silylated chalcogen reagents. Postsynthesis grafting of ethylenediamine facilitates the complexation of anhydrous zinc acetate to the pore surface via a ligand exchange process between monodentate 3,5-lutidine ligands and the anchored chelating moiety. Coordinated zinc acetate readily reacts with E(SiMe(3))(2) (E = S, Se, or Te), thereby encapsulating zinc chalcogenides in the mesoporous channels. ZnE-MCM-41 materials have been characterized by EDX analysis, nitrogen sorption analysis, and Raman, UV-vis, and solid-state NMR spectroscopy. The observed blue shift in the absorption maximum is in agreement with the expected quantum confinement of these materials given the nanometer dimensions of the mesoporous architecture of the silicate host.
通过使用硅烷化的硫属元素试剂，在室温下已成功地在MCM-41的介孔框架内制备了二元材料硫化锌（ZnS）、硒化锌（ZnSe）和碲化锌（ZnTe）。乙二胺的合成后接枝通过单齿3,5-二甲基吡啶配体与锚定的螯合部分之间的配体交换过程，促进无水醋酸锌与孔表面的络合。配位的醋酸锌很容易与E(SiMe(3))(2)（E = S、Se或Te）反应，从而将硫属锌化物封装在介孔通道中。通过能量色散X射线分析（EDX分析）、氮吸附分析以及拉曼光谱、紫外可见光谱和固态核磁共振光谱对ZnE-MCM-41材料进行了表征。鉴于硅酸盐主体介孔结构的纳米尺寸，观察到的最大吸收峰蓝移与这些材料预期的量子限域一致。
