One‐Step Synthesis of Core‐Shell‐Structured Mixed‐Metal CPO‐27(Cu,Co) and Investigations on Its Controlled Thermal Transformation

Using the mixed-metal approach, a direct synthesis route at ambient pressure was developed for a new type of bimetallic metal-organic framework based on the CPO-27 structure. The structural characterization of CPO-27(Cu$_{0.6}$−CS−Co$_{0.4}$) using X-ray diffraction, transmission electron microscopy, energy-dispersive X-ray mapping and X-ray absorption spectroscopy revealed that the Cu$^{2+}$ and Co$^{2+}$ ions were exclusively incorporated at the metal positions of the CPO-27 lattice, but with a core-shell distribution within the crystallites. The parent framework material was then utilized as a precursor for the generation of novel bimetallic carbon-supported materials using the controlled thermal decomposition in a reducing atmosphere. During this decomposition process, the distribution of the two metals remained the same, which resulted in unique needle-shaped particles with a high dispersion of cobalt at the periphery of the amorphous carbon and agglomerated copper particles in the inside