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The scattering of primary beam electrons has several implications for energy dispersive X-ray analysis on the environmental scanning electron microscope (ESEM). One of the most basic problems is determining the spatial distribution and fraction of primary beam electrons scattered under typical high pressure analysis conditions A method for studying the scattering of the primary electron beam in the ESEM has been demonstrated. The method involves the use of self-assembled alkanethiol monolayers (SAM) which are sensitive to damage by primary beam electrons. After irradiation, the electron damaged molecules can be exchanged out of the monolayer by immersion in a second alkanethiol solution. The spatial distribution of this second marker compound can then be imaged directly by static secondary ion mass spectrometry (SSIMS). Alternatively, only a single fluorinated thiol is used and the decrease in fluorine secondary ion signal is used to map the electron damage.
Polycrystalline thin films of BaTiO3 were deposited on fused quartz substrates at 600°C by metalorganic chemical vapor deposition (MOCVD). The films were characterized by x-ray powder diffraction (XRD), transmission electron microscopy (TEM), secondary ion mass spectroscopy (SIMS) and Raman spectroscopy. Films prepared in the early stages of this study that had appeared to contain only crystalline BaTiO3 by XRD were found to have nonuniform composition and microstructure through the film thickness by SIMS and TEM. The MOCVD system was then modified by installing a process gas bypass apparatus and an elevated pressure bubbler for the titanium isopropoxide precursor. A 1.2 μm thick BaTiO3 film prepared in the modified system demonstrated much improved compositional and microstructural uniformity through the thickness of the film. This film had a columnar microstructure with grain widths of 0.1–0.2 μm and exhibited tetragonality as detected by Raman spectroscopy.
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