Transmission Electron Microscopy Essay

EXPERIMENTAL SECTION

General remarks. All of the reagents and solvents were commercially available and purchased from Fluka, Merck, and Aldrich chemical companies. Transmission electron microscopy (TEM) analyse was performed using a TEM microscope Philips CM 120 KV Netherland. X-ray diffraction (XRD) patterns were obtained on Inel French, EQUINOX 3000 model X-ray diffractometer using Cu-K radiation. Scanning electron/electron backscatter diffraction microscopy (SEM)/(EBSD) has been performed using an SU3500 microscope with scanning range from 0 to 20 keV. Electron dispersive X-ray spectroscopy (EDX) measurements were made with an IXRF model 550i attached to SEM. SEM-EBSD/EDX samples were prepared by coating of solid particles into a conductive layer. Fourier transform infrared spectroscopy (FT-IR) spectra were recorded with

Typically, FeCl2.4H2O (4.3 g) and FeCl3.6H2O (11.6 g) were mixed with 350 mL of deionized water under N2 atmosphere. The resulting solution was heated to 80 °C while stirring, vigorously. Then, 20 mL of 25% NH4OH was quickly added into the solution. The resulting suspension was vigorously stirred for 5 min and then, the black precipitates were collected with the help of a magnet and washed repeatedly with deionized water and ethanol, then dried at vacuum

Firstly, 0.3 g Fe3O4 was ultrasonically dispersed into 150 ml solvent (Vmethanol/Vwater=1/1) for 20 min to obtain a uniform suspension. A 100 ml alkaline solution (0.32 g Na2CO3, 0.48 g NaOH) was added dropwise into the suspension until pH ca. 10.0 and kept for 5 min, then another 100 ml salt solution (1.02 g Mg(NO3)2⋅6H2O and 1.2 g Al(NO3)3⋅9H2O) and above alkaline solution were simultaneously added maintaining the pH in 9.5-10.0. The resultant was stirred for 5 min followed separation by using a magnet and thoroughly washing with deionized water and alcohol and dried at 60 °C overnight giving product Fe-Mg/Al