Nanosize FexOy @SBA-3: A Comparative Study Between Conventional and Microwave Assisted Synthesis

The present study is focussed on development of highly dispersed nanosize iron oxide (FexOy) particles within the uniform mesopore channels of SBA-3. Herein we report a comparative study between conventional incipient wetness and microwave assisted synthesis routes adopted to devise nanoparticles. The developed materials are characterised by following X-ray diffraction, high resolution transmission electron microscopy, proton induced X-ray emission, diffuse reflectance UV-visible spectroscopy, thermogravimetry and Fourier transform infrared spectroscopy. Mesoporous siliceous SBA-3 was prepared at room temperature to obtain samples with good crystallinity and ordered pore structure. Pore channels of SBA-3 were used as nanoreactor for developing iron oxide nanoparticles. Iron oxide nanoparticles developed under microwave activation showed uniform distribution within the SBA-3 structure along with retaining the orderness of the pore architecture. On the contrary, iron oxides developed under incipient wetness method followed by conventional heating resulted in agglomeration of nanoparticles along with significant loss in SBA-3 pore structure. Proton induced X-ray emission studies revealed the extremely high purity of the samples and almost thrice higher amount of iron oxide particles are encapsulated within the host by microwave assisted preparation as compared to incipient/conventional heating method.