Synthesis of Cu/CuO nanoparticles in mesoporous material by solid state reaction

• Incorporation of CuO in MCM-41 material by solid state reaction.
• Cu/CuO nanoparticles produced when Cu2+/MCM-41 calcined at 500 °C.
• Presence of Cu nanoparticles depends to amount of Cu2+ and calcined temperature.

The Mobil Composition of Matter No. 41 (MCM-41) containing 1.0 and 5.0 wt.% of Cu was synthesized under solid state reaction. The calcinations of samples were done at two different temperatures, 500 and 300 °C. X-ray diffraction (XRD), UV–Vis diffuse reflectance spectroscopy (UV–Vis DRS), Fourier transform infrared spectroscopy (FTIR) and transmission electron microscopy (TEM) were used for samples characterization. Powder X-ray diffraction showed that when Cu(CH3COO)2 content is about 1.0 wt.% in Cu/MCM-41, the guest CuO-NPs and copper ions is formed on the silica channel wall, and more exists in the crystalline state. When Cu(CH3COO)2 content exceeds this value (5.0 wt.%), CuO nanoparticles and Cu2+ ions can be observed in low crystalline state. From the diffuse reflectance spectra it was confirmed that 5 wt.% Cu/MCM-41 sample calcined at 500 °C show plasmon resonance band due to Cu nanoparticles in the range between 500 and 600 nm and small copper clusters Cun in 450 nm. It also shows that some of the Cu2+ ions are present octahedrally in extraframework position in all samples. Both fourier transform infrared and diffuse reflectance spectra indicate that some of Cu2+ ions are tetrahedrally within the framework position in 1 wt.% Cu/MCM-41 samples. TEM images indicated that nanoparticles size of CuO is in range of 30–40 nm.

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