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Eingeladener Vortrag
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Lateral resolution, also called image resolution, is the most relevant quality parameter of maps and line scans. Therefore well defined procedures for the determination of lateral resolution are required. In the surface analysis community different definitions of lateral resolution are in use and there is no generally accepted method for the determination of lateral resolution which meets the demands of the state-of-the-art in surface analysis. We propose the determination of lateral resolution by imaging of well defined square-wave gratings with finely graded periods. This method enables the real time estimation of lateral resolution and the adjustment of instrument settings with respect to lateral resolution. The effect of noise and contrast on lateral resolution has been analysed by numerically simulated images of square-wave gratings. A new resolution criterion has been developed which is based on the dip-to-noise ratio and takes into account the sampling step width by introducing a "reduced noise". The contrast transfer function has been introduced and its relation to lateral resolution in the presence of noise was analysed. For that reason an "effective cut-off frequency" was defined which is the reciprocal of the lateral resolution. Normalized values of lateral resolution and their relation to signal-to-noise ratio and sampling step width were given for Gaussian and Lorentzian line spread functions. These values enable the calculation of experimental parameters which are necessary to get a required value of lateral resolution. Finally the successful application of the proposed approach to determine lateral resolution has been demonstrated by ToF-SIMS element mapping of the certified reference material BAM-L200.
Time-of-flight secondary ion mass spectrometry (TOF-SIMS) mappings provide a visualization of the distribution of chemical elements and phases on polished duplex steel surfaces as element and fragment secondary ion signals. The advantage of TOF-SIMS, compared to optical microscopy, is its potential to analyze the chemical composition with a lateral resolution at a submicrometer scale. TOF-SIMS mappings allow distinguishing between ferritic and austenitic phases because of the phase selective detection method without any requirement of etching or other processing.
Recently, time-of-flight secondary ion mass spectrometry (ToF-SIMS) and X-ray photoelectron spectroscopy (XPS) instrumentation has been used to address areas of interest within micro-fluidic devices providing full access to the surface chemistry established at the bottom of micro-channels therein. After careful calibration, information on surface chemistry as obtained by ToF-SIMS or XPS can be interpreted in terms of wettability expressed as contact angles which are then characteristic for the inner walls of micro-channels. Standard contact angle measurement is not applicable in micro-channels. The approach has been demonstrated to be successful with two different micro-fluidic devices hot embossed into high-end quality poly(methyl methacrylate) (PMMA) or Polycarbonate wafers. A pre-selected surface chemistry at micro-channel walls can be established by plasma technologies but ageing and rinsing effects have to be under control. A combination of ToF-SIMS, XPS and contact angle measurement techniques has been demonstrated to provide the required information. Finally, it is shown by ToF-SIMS and XPS analysis that in the production of micro-fluidic parts during practical processing using hot embossing technologies, material originating from cover foils will reside on the polymer wafer's surface. Moreover, residues of releasing agents as silicone oil used during processing can be detected by ToF-SIMS. Both cover foil residues and silicones are issues of trouble shooting in micro-fluidics because they will change contact angles efficiently.
A first inter-laboratory comparison was conducted to demonstrate and document the capability of interested laboratories to measure the fraction of C—OH species on a plasma oxidised poly(propylene) sample by using a chemical derivatisation XPS approach. This report presents the results from that inter-laboratory comparison and includes the data received for the measured values and their associated standard deviations of laboratory means, at a 95% confidence level. The measurements were guided by a protocol developed within the group before and summarised shortly in the paper. Standard deviations that may characterise the state-of-the-art for the nominally simple and rather often practised case of TFAA chemical derivatisation XPS of C—OH species on a plasma oxidised polyolefin surface are calculated following ISO 5725-2:1994. The main conclusion is that the associated degree of equivalence reached by the participating laboratories in this comparison is still low. Further research to improve chemical derivatisation XPS protocols is mandatory.