MRI: Acquisition of a small angle X-ray diffractometer for in situ measurements of liquid to solid samples over a wide range of temperatures Mark A. Snyder,

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MRI: Acquisition of a small angle X-ray diffractometer for in situ measurements of liquid to solid samples over a wide range of temperatures Mark A. Snyder, Lehigh University, DMR M ILESTONE : I NSTRUMENT COMMISSIONING (2/27/2015) This MRI has supported the acquisition and commissioning of a uniquely configured SAXSpace (Anton Paar® GmbH) small-angle X-ray scattering (SAXS) instrument (A) that has simultaneous and continuous wide-angle X- ray diffraction (XRD) capabilities (B) and a multi-collimated (line (B,E,F), point (C,D)) high-flux X-ray beam suitable for probing a diverse range of weakly scattering isotropic and anisotropic samples. I NSTRUMENT C APABILITIES The instrument has been uniquely configured to address a diverse range of research needs of PIs within Lehigh as well as at regional colleges and industrial partners. In addition to sample stages enabling analysis of powders (B,D,E), solutions (i.e., capillary measurements, E), gels, viscous or flowing liquids, and small (10  L) volume high-value solutions, we have configured the instrument with multiple modular characterization capabilities, including a temperature stage enabling measurements from -150 o C to 300 o C, an in situ tensile stage with two load cells (5 N, 600 N), and a grazing incidence (GI) stage enabling both GI-SAXS and GI-XRD on structured thin films (D). I NTELLECTUAL M ERIT On Lehigh’s campus, the instrument promises to capitalize on the complementarity of SAXS/WAXS with existing state-of- the-art electron microscopy, spectroscopy, and proximal probe facilities to enhance active research spanning: (i) functional, mesostructured and mesoporous inorganic materials, (ii) organic, inorganic, and hybrid films, buried interfaces, and (iii) biological and hybrid materials, in applications as diverse as catalysts for biomass-to-chemicals conversion, photocatalysts for low-cost liquid fuel production, bioactive glass scaffolding for hard tissue regeneration, mechanics of biomimetic materials and multi- functional nanocomposites, protein and cell membrane phase behavior for biomimetic toxin sensing, and novel therapeutics design, among others. Figure showing (A) the newly commissioned SAXSpace instrument and representative initial scattering measurements collected on the instrument under various configurations and for various sample types, including SAXS/WAXS (B) line- and (C,C1) point-collimated powder measurements and (D) GI-SAXS/GI-WAXS film measurements of crystalline silver behenate standards, as well as line-collimated measurements of (E) silica nanoparticle (50 nm) crystalline assemblies and (F,F1) capillary measurements of aqueous silica nanoparticle (20 nm) dispersions.

MRI: Acquisition of a small angle X-ray diffractometer for in situ measurements of liquid to solid samples over a wide range of temperatures Mark A. Snyder, Lehigh University, DMR E ARLY B ROADER I MPACT During the instrument commissioning, a public 1 hour interactive seminar was organized and aimed at a basic introduction of small-angle X-ray scattering theory, exposure to example SAXS/WAXS analysis and applications, and overview of specific capabilities of Lehigh’s newly installed SAXSpace instrument. An interdisciplinary group of 50+ faculty, graduate students, and postdocs spanning Chemical and Biomolecular Engineering, Materials Science and Engineering, Mechanical Engineering, Bioengineering, Chemistry, Earth and Environmental Science, and Physics attended. Interested attendees were provided with the copies of H. Schnablegger & Y. Singh, “The SAXS Guide,” 3 rd Ed., Anton Paar GmbH (2013). The seminar was digitally archived, and will be made available through a dedicated instrument website for future users and college courses. H ANDS - ON T RAINING AND SAXS PACE D EMONSTRATIONS Two, 3-hour interactive workshops were conducted for ~30 faculty, postdoctoral researchers, and students during the instrument commissioning. These included hands-on sample preparation techniques, data collection, and discussion of SAXS data classification. B ROAD, I NTERDISCIPLINARY R EGIONAL U SER B ASE The modular nature of the instrument will help advance research of a diverse, multi-disciplinary user group including more than 32 faculty and their graduate students, postdoctoral researchers, and undergraduates at Lehigh University and at least 4 regional non-PhD granting institutions. It will also service more than 9 regional industrial partners. F UTURE B ROADER I MPACT E FFORTS Development and deployment of complementary interactive educational X-ray modules will impact domestic and international students in Lehigh’s Microscopy Summer School and a range of middle school, high school, and undergraduate students in educational outreach programs at Lehigh.