Study on the synthesis and structural characterization of spinel-structured Co3O4 metal oxide derived from metal-organic framework materials
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https://doi.org/10.54939/1859-1043.j.mst.113.2026.81-87Keywords:
Spinel structure; Co3O4; Metal-organic framework; XRD; EDX; FTIR; SEM; BET.Abstract
Spinel Co3O4 materials were successfully synthesized through the thermal decomposition of Co-BTC metal-organic frameworks prepared by hydrothermal and microwave-assisted methods. The structural characteristics and physicochemical properties of the materials were investigated by XRD, EDX, FTIR, SEM, and N₂ adsorption-desorption analyses. XRD and FTIR results confirmed the complete transformation of Co-BTC into pure spinel Co3O4 with high crystallinity, while EDX analysis indicated the complete removal of organic components after calcination. SEM images revealed that Co-BTC exhibited rod-like crystals, whereas Co3O4 consisted of near-spherical nanoparticles with sizes of approximately 50-60 nm, forming a porous structure. All samples exhibited mesoporous characteristics with type IV-H3 adsorption isotherms. The Co3O4 sample derived from the microwave-assisted MOF precursor achieved the highest specific surface area of 80.1 m2/g, which was significantly higher than that of the hydrothermal sample. The microwave-assisted method reduced the synthesis time to 60 min while improving the porous structure and process efficiency in accordance with green chemistry principles.
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