DOE OSTI2012
Quantification of synchrotron XRF analyses is typically done through comparisons with measurements on the NIST SRM 1832/1833 thin film standards. Unfortunately, these standards are inhomogeneous on small scales at the tens of percent level. We are synthesizing new homogeneous multilayer standards using the Atomic Layer Deposition technique and characterizing them using multiple analytical methods, including ellipsometry, Rutherford Back Scattering at Evans Analytical, Synchrotron X-ray Fluorescence (SXRF) at Advanced Photon Source (APS) Beamline 13-ID, Synchrotron X-ray Absorption Spectroscopy (XAS) at Advanced Light Source (ALS) Beamlines 11.0.2 and 5.3.2.1 and by electron microscopy techniques. Our motivation for developing much-needed cross-calibration of synchrotron techniques is borne from coordinated analyses of particles captured in the aerogel of the NASA Stardust Interstellar Dust Collector (SIDC). The Stardust Interstellar Dust Preliminary Examination (ISPE) team have characterized three sub-nanogram, {approx}1{micro}m-sized fragments considered as candidates to be the first contemporary interstellar dust ever collected, based on their chemistries and trajectories. The candidates were analyzed in small wedges of aerogel in which they were extracted from the larger collector, using high sensitivity, high spatial resolution >3 keV synchrotron x-ray fluorescence spectroscopy (SXRF) and <2 keV synchrotron x-ray transmission microscopy (STXM) during Stardust ISPE. The ISPE synchrotron techniques have complementary capabilities. Hard X-ray SXRF is sensitive to sub-fg mass of elements Z {ge} 20 (calcium) and has a spatial resolution as low as 90nm. X-ray Diffraction data were collected simultaneously with SXRF data. Soft X-ray STXM at ALS beamline 11.0.2 can detect fg-mass of most elements, including cosmochemically important oxygen, magnesium, aluminum and silicon, which are invisible to SXRF in this application. ALS beamline 11.0.2 has spatial resolution better than 25 nm. Limiting factors for Stardust STXM analyses were self-imposed limits of photon dose due to radiation damage concerns, and significant attenuation of <1500 eV X-rays by {approx}80{micro}m thick, {approx}25 mg/cm{sup 3} density silica aerogel capture medium. In practice, the ISPE team characterized the major, light elements using STXM (O, Mg, Al, Si) and the heavier minor and trace elements using SXRF. The two data sets overlapped only with minor Fe and Ni ({approx}1% mass abundance), providing few quantitative cross-checks. New improved standards for cross calibration are essential for consortium-based analyses of Stardust interstellar and cometary particles, IDPs. Indeed, they have far reaching application across the whole synchrotron-based analytical community. We have synthesized three ALD multilayers simultaneously on silicon nitride membranes and silicon and characterized them using RBS (on Si), XRF (on Si{sub 3}N{sub 4}) and STXM/XAS (holey Si{sub 3}N{sub 4}). The systems we have started to work with are Al-Zn-Fe and Y-Mg-Er. We have found these ALD multi-layers to be uniform at {micro}m- to nm scales, and have found excellent consistency between four analytical techniques so far. The ALD films can also be used as a standard for e-beam instruments, eg., TEM EELS or EDX. After some early issues with the consistency of coatings to the back-side of the membrane windows, we are confident to be able to show multi-analytical agreement to within 10%. As the precision improves, we can use the new standards to verify or improve the tabulated cross-sections.
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