Browsing by Subject "Charging property"

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Open Access
Analysis of Fe nanoparticles using XPS measurements under d.c. or pulsed-voltage bias
(2010) Süzer, Şefik; Baer, D. R.; Engelhard, M. H.
The impact of solution exposure on the charging properties of oxide coatings on Fe metal-core oxide-shell nanoparticles has been examined by sample biasing during XPS measurements. The Fe nanoparticles were suspended in relatively unreactive acetone and analyzed after particles containing solutions were deposited on SiO2/Si or Au substrates. The particle and substrate combinations were subjected to ±10V d.c. or ±5V a.c., biasing in the form of square wave (SQW) pulses. The samples experienced variable degrees of charging for which low-energy electrons at ∼1eV, 20 μA and low-energy Ar+ ions were used to minimize it. Application of d.c. bias and/or SQW pulses significantly influences the extent of charging, which is utilized to gather additional analytical information about the sample under investigation. This approach allows separation of otherwise overlapping peaks. Accordingly, the O1s peaks of the silicon oxide substrate, the iron oxide nanoparticles, and that of the casting solvent can be separated from each other. Similarly, the C1s peak belonging to the solvent can be separated from that of the adventitious carbon. The charging shifts of the iron nanoparticles are strongly influenced by the solvent to which the particles were exposed. Hence, acetone exhibited the largest shift, water the smallest, and methanol in between. Dynamical measurements performed by application of the voltage stress in the form of SQW pulses provides information about the time constants of the processes involved, which leads us to postulate that these charging properties we probe in these systems stem mainly from ionic movement(s).
Open Access
Methods for probing charging properties of polymeric materials using XPS
(2010) Sezen, H.; Ertas, G.; Süzer, Şefik
Various thin polystyrene, PS, and poly(methyl methacrylate), PMMA and PS + PMMA blend films have been examined using the technique of recording X-ray photoelectron spectrum while the sample is subjected to ±10 V d.c. bias, and three different forms of (square-wave (SQW), sinusoidal (SIN) and triangular (TRG)), a.c. pulses. All films exhibit charging shifts as observed in the position of the corresponding C1s peak under d.c. bias. The a.c. pulses convert the single C1s peak to twinned peaks in the case of the square-wave form, and distort severely in the cases of the SIN, and TRG forms, and all three of them exhibit strong frequency dependence. In order to mimic and better understand the behavior of these polymeric materials, an artificial dielectric system consisting of a clean Si-wafer coupled to an external 1 MΩ resistor and 56 nF capacitor is created, and its response to different forms of voltage stimuli, is examined in detail. A simple electrical circuit model is also developed treating the system as consisting of a parallel resistor and a series capacitor. With the help of the model, the response of the artificial system is successfully calculated as judged by comparison with the experimental data. Using one high frequency SQW measurements, the off-set in the charging shift due to the extra low-energy neutralizing electrons is estimated. After correcting the corresponding off-set shifts, the XPS spectra of the three different PS films, one PMMA, and one PS + PMMA blend film are re-examined. As a result of these detailed analysis, there emerges a clear relationship between the thicknesses of the PS films with their charging abilities. In the blend film, PS and PMMA domains are electrically separated, and exhibit different charging shifts, however, the presence of one is felt by the other. Hence, the PS component shifts are larger in the blend, due to the presence of PMMA domains, which has intrinsically a larger Reff, and conversely the PMMA component shifts are smaller due to the presence of PS domains.