Kowalchuk Collin M, Schmid Günter, Meyer-Zaika Wolfgang, Huang Yining, Corrigan John F
Department of Chemistry, The University of Western Ontario, London Ontario, N6A 5B7 Canada.
Inorg Chem. 2004 Jan 12;43(1):173-80. doi: 10.1021/ic0300868.
The copper-tellurolate cluster [(Cu(6)(TePh)(6)(PPh(2)Et)(5)] has been loaded into the pores of MCM-41 by solid-state impregnation techniques. It was found that the best loading conditions are 110 degrees C and 10(-)(3) Torr static vacuum. The resulting material was analyzed by powder X-ray diffraction (PXRD), nitrogen adsorption isotherms, thermogravimetric analysis (TGA), (31)P CP MAS NMR spectroscopy, and TEM. It was observed that loading is accompanied by loss of the phosphine shell, with retention of the copper-tellurium core. Condensation of the impregnated material may proceed thermally or photochemically. Thermal condensation results in the formation of Cu(2)Te nanoparticles as demonstrated by PXRD, and TEM data suggests that the process has taken place inside the pores of MCM-41. Photochemical condensation yields larger metal-chalcogen clusters in the pores as suggested by the result of UV-vis diffuse reflectance spectroscopy and TEM measurements.
通过固态浸渍技术将碲化铜簇合物[(Cu(6)(TePh)(6)(PPh(2)Et)(5)]载入MCM - 41的孔中。发现最佳载入条件为110℃和10⁻³托的静态真空。通过粉末X射线衍射（PXRD）、氮吸附等温线、热重分析（TGA）、³¹P CP MAS NMR光谱和透射电子显微镜（TEM）对所得材料进行分析。观察到载入过程伴随着膦壳的损失，而铜 - 碲核得以保留。浸渍材料的缩合反应可通过热或光化学方式进行。热缩合导致形成Cu₂Te纳米颗粒，这由PXRD证明，并且TEM数据表明该过程发生在MCM - 41的孔内。紫外 - 可见漫反射光谱和TEM测量结果表明，光化学缩合在孔中产生更大的金属 - 硫族元素簇。
