According to the results of powder X-ray diffraction study of the complex salts of composition [M(NH3)(5)Cl][M'Cl-4] (M = Ir, Rh, or Co and M' = Pt or Pd), the anhydrous salts crystallize in the orthorhombic system (space group Pnma) and are isostructural to the [Ir(NH3)(5)Cl][PtCl4] complex studied previously. The unit cell parameters of the resulting salts were refined. The metal powders, which were obtained by thermal decomposition of these salts under an atmosphere of hydrogen, were studied by powder X-ray analysis.
纳米合金,特别是纳米多孔合金的潜在优势,使它们成为多相催化的“聚光灯”。尽管如此,控制这些材料的精确成分仍然是一个综合挑战。先前的研究介绍了通过氢介导的金属络盐化学还原过程来制造具有高纳米级孔隙率和可控成分的金属和合金。我们已经使用这个程序获得了两种磁性纳米多孔 Co-Pd 合金,纯多孔钯和纯多孔钴。单晶 X 射线衍射研究能够确定用作这些合金前体的两种 Co-Pd 双络合物盐的结构。粉末 X 射线衍射研究确定了合金的结晶相并表明了其微晶的纳米尺寸。高分辨率扫描电子显微镜表明,这些合金组装为相互连接的纳米微晶的高度多孔簇。它还表明,每个合金簇都保留了其盐前体的微米形态。能量色散 X 射线光谱表明,合金在微观水平上表现出均匀的成分,从而保持了盐中的 Co/Pd 比率。聚焦离子束断层扫描可实现合金和金属的 3D 结构表示。3D 重建数据的几何分析确定了 90% 的孔隙率和 ~100 m 的比表面积