White Light Interferometry for Quantitative Surface Characterization in Ion Sputtering Experiments

White light interferometry (WLI) can be used to obtain surface morphology information on dimensional scale of millimeters with lateral resolution as good as ~1 {\mu}m and depth resolution down to 1 nm. By performing true three-dimensional imaging of sample surfaces, the WLI technique enables accurate quantitative characterization of the geometry of surface features and compares favorably to scanning electron and atomic force microscopies by avoiding some of their drawbacks. In this paper, results of using the WLI imaging technique to characterize the products of ion sputtering experiments are reported. With a few figures, several example applications of the WLI method are illustrated when used for (i) sputtering yield measurements and time-to-depth conversion, (ii) optimizing ion beam current density profiles, the shapes of sputtered craters, and multiple ion beam superposition and (iii) quantitative characterization of surfaces processed with ions. In particular, for sputter depth profiling experiments of 25Mg, 44Ca and 53Cr ion implants in Si (implantation energy of 1 keV per nucleon), the depth calibration of the measured depth profile curves determined by the WLI method appeared to be self-consistent with TRIM simulations for such projectile-matrix systems. In addition, high depth resolution of the WLI method is demonstrated for a case of a Genesis solar wind Si collector surface processed by gas cluster ion beam: a 12.5 nm layer was removed from the processed surface, while the transition length between the processed and untreated areas was 150 {\mu}m.Comment: Applied Surface Science, accepted: 7 pages and 8 figure

Steps toward accurate large-area analyses of Genesis solar wind samples: evaluation of surface cleaning methods using total reflection X-ray fluorescence spectrometry

Total reflection X-ray fluorescence spectrometry (TXRF) was used to analyze residual surface contamination on Genesis solar wind samples and to evaluate different cleaning methods. To gauge the suitability of a cleaning method, two samples were analyzed following cleaning by lab-based TXRF. The analysis comprised an overview and a crude manual mapping of the samples by orienting them with respect to the incident X-ray beam in such a way that different regions were covered. The results show that cleaning with concentrated hydrochloric acid and a combination of hydrochloric acid and hydrofluoric acid decreased persistent inorganic contaminants substantially on one sample. The application of CO2 snow for surface cleaning tested on the other sample appears to be effective in removing one persistent Genesis contaminant, namely germanium. Unfortunately, the TXRF analysis results of the second sample were impacted by relatively high background contamination. This was mostly due to the relatively small sample size and that the solar wind collector was already mounted with silver glue for resonance ion mass spectrometry (RIMS) on an aluminium stub. Further studies are planned to eliminate this problem. In an effort to identify the location of very persistent contaminants, selected samples were also subjected to environmental scanning electron microscopy. The results showed excellent agreement with TXRF analysis

Steps Toward Accurate Large Area Analyzes of Genesis Solar Wind Samples: Evaluation of Surface Cleaning Methods Using Total Reflection X-ray Fluorescence Spectrometry

Total reflection X-ray fluorescence spectrometry (TXRF) was used to analyze residual surface contamination on Genesis solar wind samples and to evaluate different cleaning methods. The Genesis mission collected solar wind during a period of 854 days by embedding the charged particles into collectors made of various ultra clean materials such as silicon, sapphire and silicon-on-sapphire. The sample return capsule unexpectedly crashed on return to Earth fracturing the collectors and exposing them to the desert soil of the landing side. The ubiquitous contaminants are separated from the atoms of solar wind by only 5-15 nm, presenting significant challenges for solar wind analysis as well as the development of cleaning techniques. Currently, an ultrapure water and ozone UV radiation treatment is routinely applied to the collectors by the curatorial team at NASA’s Johnson Space Center. Additional cleaning steps involving various forms of acid treatment and/or carbon dioxide snow treatment are being evaluated as well. To gauge the suitability of the cleaning method, two samples were analyzed following cleaning by lab-based TXRF. The analysis comprised of an overview and a crude manual mapping of the samples by orienting them with respect to the incident X-ray beam in such way that different regions were covered. The results showed that cleaning with concentrated hydrochloric acid and a combination of hydrochloric acid and hydrofluoric acid decreased persistent inorganic contaminants substantially on one sample. Application of carbon dioxide snow for surface cleaning tested on the other sample appears to be effective in removing one persistent Genesis contaminant, namely germanium. Unfortunately, the TXRF analysis results of the second sample were impacted by relatively high background contamination. This was mostly due to the relatively small sample size and that the solar wind collector was already mounted with silver glue for resonance ion mass spectrometry (RIMS) on an aluminum stub. Further studies are planned to eliminate this problem. In an effort to identify the location of very persistent contaminants, selected samples were also subjected to environmental scanning electron microscopy. The results showed excellent agreement with TXRF analysis