XTOP 2018 - the 14th Biennial Conference on High-Resolution X-Ray Diffraction and Imaging Bari, 3rd -7th September 2018 TABLE-TOP SCANNING SAXS/WAXS MICROSCOPY OF ENGINEERED NANO/BIO-MATERIALS D. Altamura1,*, S.G. Pastore1, D. Siliqi1, M. Ladisa1, F. Scattarella1, A. Terzi1, and C. Giannini1 1 CNR-Istituto di Cristallografia, Via Amendola 122/O, 70126 Bari, Italy *e-mail: (davide.altamura@ic.cnr.it) INTRODUCTION: Simultaneous SAXS/WAXS data collection allows to directly relate atomic and nano- scale structures at each point on the sample. Synchrotron beamlines typically exploit an off-axis detector for WAXS, although this prevents the collection of diffraction rings over the full azimuthal range, or scanning is performed twice to collect the full scattering signal at small (SAXS) and wide (WAXS) angles. Despite the excellent data quality, a possible drawback can be some information loss and/or mismatch between SAXS and WAXS maps due to sample structural evolution (spontaneous, due to drying, radiation damage, drifts). A different approach, also available in table-top facilities, exploits an image plate detector with central hole, to collect the average 2D WAXS signal along with a spatially resolved SAXS map, and/or single SAXS/WAXS patterns from selected sample points. EXPERIMENTAL: A Rigaku synchrotron-class micro-source, coupled to a SAXS/WAXS camera, allows for double length scale diffraction microscopy with 70?200 ?m spatial resolution1. RESULTS AND DISCUSSION: Even though a scattering component from sample local structure can be partially smeared out in the integrated average, the spatially resolved SAXS/Absorption map can help in discriminating and localizing micro- and nano-scale components (e.g. CaS and HA, respectively, in the Figure), through the following simultaneous SAXS/WAXS signal collection from selected regions of interest. Once the correspondence of SAXS/WAXS features is assessed, the 2D SAXS/Absorption map can be used for qualitative structural mapping, quantitative estimation of concentration gradients (e.g. HA nanocrystals across the scaffold in the Figure)1, or statistical quantitative information can be extracted by averaging the normalized SAXS intensity in selected q-ranges, for comparative studies on nanoparticle abundance (e.g. oil nanodroplets in films made from emulsions)2, among others. CONCLUSIONS: The simultaneous SAXS/WAXS-integrated full pattern collection allows for double length scale description of the real-time status of the sample, with 2D spatial resolution, without loss of intensity or possibly information in case of preferred orientations, and is feasible with laboratory equipment. REFERENCES: 1. D. Altamura, S. G. Pastore, M. G. Raucci, D. Siliqi, F. De Pascalis, M. Nacucchi, L. Ambrosio, and C. Giannini. ACS Appl. Mater. Interfaces (2016), 8, 8728-8736. 2. Juan M. Montes de Oca-Ávalosa, D. Altamura, Roberto J. Candal, F. Scattarella, D. Siliqi, C. Giannini, M. Lidia Herrera. Relationship between nano/micro structure and physical properties of TiO2-sodium caseinate composite films. Food research international (2018), 105, 129-139. ACKNOWLEDGEMENTS: M.G. Raucci, I. Fasolino and L. Ambrosio (CNR-IPCB) are aknowledged for providing cell seeded scaffolds. D. Mele and F. Intranuovo (University of Bari) are aknowledged for support with micro-CT. E. Altamura and F. Mavelli (University of Bari) are aknowledged for confocal microscopies. R. Lassandro (CNR-IC) is acknowledged for his technical support in the XMI-Lab.
Table-Top Scanning SAXS/WAXS Microscopy of Engineered Nano/Bio-Materials
D Altamura;D Siliqi;M Ladisa;F Scattarella;A Terzi;C Giannini
2018
Abstract
XTOP 2018 - the 14th Biennial Conference on High-Resolution X-Ray Diffraction and Imaging Bari, 3rd -7th September 2018 TABLE-TOP SCANNING SAXS/WAXS MICROSCOPY OF ENGINEERED NANO/BIO-MATERIALS D. Altamura1,*, S.G. Pastore1, D. Siliqi1, M. Ladisa1, F. Scattarella1, A. Terzi1, and C. Giannini1 1 CNR-Istituto di Cristallografia, Via Amendola 122/O, 70126 Bari, Italy *e-mail: (davide.altamura@ic.cnr.it) INTRODUCTION: Simultaneous SAXS/WAXS data collection allows to directly relate atomic and nano- scale structures at each point on the sample. Synchrotron beamlines typically exploit an off-axis detector for WAXS, although this prevents the collection of diffraction rings over the full azimuthal range, or scanning is performed twice to collect the full scattering signal at small (SAXS) and wide (WAXS) angles. Despite the excellent data quality, a possible drawback can be some information loss and/or mismatch between SAXS and WAXS maps due to sample structural evolution (spontaneous, due to drying, radiation damage, drifts). A different approach, also available in table-top facilities, exploits an image plate detector with central hole, to collect the average 2D WAXS signal along with a spatially resolved SAXS map, and/or single SAXS/WAXS patterns from selected sample points. EXPERIMENTAL: A Rigaku synchrotron-class micro-source, coupled to a SAXS/WAXS camera, allows for double length scale diffraction microscopy with 70?200 ?m spatial resolution1. RESULTS AND DISCUSSION: Even though a scattering component from sample local structure can be partially smeared out in the integrated average, the spatially resolved SAXS/Absorption map can help in discriminating and localizing micro- and nano-scale components (e.g. CaS and HA, respectively, in the Figure), through the following simultaneous SAXS/WAXS signal collection from selected regions of interest. Once the correspondence of SAXS/WAXS features is assessed, the 2D SAXS/Absorption map can be used for qualitative structural mapping, quantitative estimation of concentration gradients (e.g. HA nanocrystals across the scaffold in the Figure)1, or statistical quantitative information can be extracted by averaging the normalized SAXS intensity in selected q-ranges, for comparative studies on nanoparticle abundance (e.g. oil nanodroplets in films made from emulsions)2, among others. CONCLUSIONS: The simultaneous SAXS/WAXS-integrated full pattern collection allows for double length scale description of the real-time status of the sample, with 2D spatial resolution, without loss of intensity or possibly information in case of preferred orientations, and is feasible with laboratory equipment. REFERENCES: 1. D. Altamura, S. G. Pastore, M. G. Raucci, D. Siliqi, F. De Pascalis, M. Nacucchi, L. Ambrosio, and C. Giannini. ACS Appl. Mater. Interfaces (2016), 8, 8728-8736. 2. Juan M. Montes de Oca-Ávalosa, D. Altamura, Roberto J. Candal, F. Scattarella, D. Siliqi, C. Giannini, M. Lidia Herrera. Relationship between nano/micro structure and physical properties of TiO2-sodium caseinate composite films. Food research international (2018), 105, 129-139. ACKNOWLEDGEMENTS: M.G. Raucci, I. Fasolino and L. Ambrosio (CNR-IPCB) are aknowledged for providing cell seeded scaffolds. D. Mele and F. Intranuovo (University of Bari) are aknowledged for support with micro-CT. E. Altamura and F. Mavelli (University of Bari) are aknowledged for confocal microscopies. R. Lassandro (CNR-IC) is acknowledged for his technical support in the XMI-Lab.I documenti in IRIS sono protetti da copyright e tutti i diritti sono riservati, salvo diversa indicazione.
