i synthesis iron oxide nanoparticles using thermal decomposition method which later stabilized in toluene. may i know, how i could characterize the phases and crystalline properties by using XRD effectively? typically XRD in my university can only handle samples in powder form. i did attempt to remove the toluene from the samples but it doesn't work. kindly advice.
Dear Mohamed :
For XRD you had to obtain a powder after thermal decomposition. Wash the impurities, centrifuge, dry. You can determine the size of the nanoparticles in toluene by SAXS or DLS. Remove the toluene by evaporation, distillation. Iron oxides are resistant to heat
Best regards/
In colloidal form the best method to determine the size is by DLS(Dynamic Light scattering) and Zeta Sizer.
For XRD Dry your sample in Vacuum or under Argon Atmosphere so that impure phases will not form
No one can perform powder diffraction measurements for phase analysis of liquids.
It is possible to dry the toluene (drying cabinet, desiccator plus vacuum pump).
You may also use TEM to characterise the sample and also the crystal structure.
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