*3.2. Methods Used to Characterize Samples*

A Philips 1830 PAnalytical X-Ray Diffractometer (Almelo, The Netherlands), using a copper source, KĮ of 1.54 Å was employed for the analysis of the crystalline components of the samples. The powders were positioned into a silicon zero background sample holder and the diffraction patterns recorded between 5° and 70° (2ș) with 0.020° step size and one second per step.

A JEOL (Tokyo, Japan) 2010F FASTEM field emission gun scanning transmission electron microscope (STEM/TEM) equipped with Gatan (Pleasanton, *CA*, USA) GIF image filtering system was used to collect images and electron diffraction patterns. The samples were dispersed in ethanol and a drop of the mixture was allowed to dry in a Holey carbon copper grid. The JEOL 2010F lattice resolution is 0.1 nm.

The microstructural features of the specimens post treatment were analyzed using a Zeiss Neon (Oberkochen, Germany) 40 High Resolution Scanning Electron Microscope (SEM). Images were acquired at diverse magnifications while the microscope was operated between 5 and 20 kV. Energy Dispersive Spectroscopy (EDS) experiments were conducted in conjunction with the SEM using an Apollo 10 silicon drift detector (SDD). Data was collected and analyzed using Genesis Spectrum software (EDAX, Mahwah, NJ, USA).

Brunauer Emmet Teller (BET) surface area analysis was performed employing a Quantachrome (Boynton Beach, *FL*, USA) Nova 4200 Physisorption analyzer. A degas step was conducted prior to the analysis. The measurements were done using nitrogen atmosphere.
