Transmission Electron Microscopy Lab Report

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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
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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…show more content…
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
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