Integrated Three-Dimensional Microanalysis Combining X-Ray Microtomography and X-Ray Fluorescence Methodologies.

A novel 3D elemental and morphological analysis approach is presented combining X-ray computed tomography (μCT), X-ray fluorescence (XRF) tomography, and confocal XRF analysis in a single laboratory instrument (Herakles). Each end station of Herakles (μCT, XRF-CT, and confocal XRF) represents the state-of-the-art of currently available laboratory techniques. The integration of these techniques enables linking the (quantitative) spatial distribution of chemical elements within the investigated materials to their three-dimensional (3D) internal morphology/structure down to 1-10 μm resolution level, which has not been achieved so-far using laboratory X-ray techniques. The concept of Herakles relies strongly on its high precision (around 100 nm) air-bearing motor system that connects the different end-stations, allowing combined measurements based on the above X-ray techniques while retaining the coordinate system. In-house developed control and analysis software further ensures a smooth integration of the techniques. Case studies on a Cu test pattern, a Daphnia magna model organism and a perlite biocatalyst support material demonstrate the attainable resolution, elemental sensitivity of the instrument, and the strength of combining these three complementary methodologies.

[1]  Bart Vekemans,et al.  Three-dimensional trace element analysis by confocal X-ray microfluorescence imaging. , 2004, Analytical chemistry.

[2]  Stefan Vogt,et al.  Hard X-ray fluorescence tomography--an emerging tool for structural visualization. , 2010, Current opinion in structural biology.

[3]  A. Rashad A synopsis about perlite as building material – A best practice guide for Civil Engineer , 2016 .

[4]  Bert Masschaele,et al.  Three-dimensional elemental imaging by means of synchrotron radiation micro-XRF: developments and applications in environmental chemistry , 2008, Analytical and bioanalytical chemistry.

[5]  P. Bruyndonckx,et al.  Laboratory 3D Micro‐XRF/Micro‐CT Imaging System , 2011 .

[6]  Laurence Lemelle,et al.  3D chemical imaging based on a third-generation synchrotron source , 2010 .

[7]  K. Nugent,et al.  Nanoscale Fresnel coherent diffraction imaging tomography using ptychography. , 2012, Optics express.

[8]  Bert Masschaele,et al.  Dual detection X-ray fluorescence cryotomography and mapping on the model organism Daphnia magna , 2010, Powder Diffraction.

[9]  P. Withers,et al.  Non-destructive mapping of grain orientations in 3D by laboratory X-ray microscopy , 2015, Scientific Reports.

[10]  Colin R. Janssen,et al.  Laboratory Scale X-ray Fluorescence Tomography: Instrument Characterization and Application in Earth and Environmental Science. , 2016, Analytical chemistry.

[11]  J. C. Elliott,et al.  X‐ray microtomography , 1982, Journal of microscopy.

[12]  M. Gabrovska,et al.  Perlite as a potential support for nickel catalyst in the process of sunflower oil hydrogenation , 2015, Russian Journal of Physical Chemistry A.

[13]  Zhenjun Wu,et al.  Performance evaluation of a slow-release packing material-embedded functional microorganisms for biofiltration , 2017, Environmental technology.

[14]  G. Silversmit,et al.  Multi-disciplinary characterization and monitoring of sandstone (Kandla Grey) under different external conditions , 2013 .

[15]  Veerle Cnudde,et al.  High-resolution X-ray computed tomography in geosciences: A review of the current technology and applications , 2013 .

[16]  Andrew W. Stevenson,et al.  In-Line Phase-Contrast X-ray Imaging and Tomography for Materials Science , 2012, Materials.

[17]  Manuel Dierick,et al.  High spectral and spatial resolution X-ray transmission radiography and tomography using a Color X-ray Camera. , 2014, Nuclear instruments & methods in physics research. Section A, Accelerators, spectrometers, detectors and associated equipment.

[18]  C. Schroer Reconstructing x-ray fluorescence microtomograms , 2001 .

[19]  Dan Sun,et al.  Utilization of paraffin/expanded perlite materials to improve mechanical and thermal properties of cement mortar , 2015 .

[20]  Veerle Cnudde,et al.  Three-dimensional phase separation and identification in granite , 2011 .

[21]  K. Nugent,et al.  Fresnel coherent diffractive imaging tomography of whole cells in capillaries , 2014 .

[22]  P. Withers,et al.  Quantitative X-ray tomography , 2014 .

[23]  Colin R. Janssen,et al.  Mechanisms of chronic waterborne Zn toxicity in Daphnia magna. , 2006, Aquatic toxicology.

[24]  P. Cloetens,et al.  New opportunities for 3D materials science of polycrystalline materials at the micrometre lengthscale by combined use of X-ray diffraction and X-ray imaging , 2009 .

[25]  Cnudde Veerle,et al.  Multi-disciplinary characterisation of a sandstone surface crust. , 2009, The Science of the total environment.

[26]  N. Cordes,et al.  Non-destructive elemental quantification of polymer-embedded thin films using laboratory based X-ray techniques , 2014 .

[27]  P. Withers,et al.  3D chemical imaging in the laboratory by hyperspectral X-ray computed tomography , 2015, Scientific Reports.

[28]  F. Brenker,et al.  X-ray Fluorescence Nanotomography on Cometary Matter from Comet 81P/Wild2 Returned by Stardust , 2009 .

[29]  E. Kapeluszna,et al.  Utilization of waste expanded perlite as new effective supplementary cementitious material , 2017 .

[30]  D. Wildenschild,et al.  X-ray imaging and analysis techniques for quantifying pore-scale structure and processes in subsurface porous medium systems , 2013 .

[31]  J. Buffière,et al.  Three-dimensional grain mapping by x-ray diffraction contrast tomography and the use of Friedel pairs in diffraction data analysis. , 2009, The Review of scientific instruments.

[32]  Paul Seller,et al.  Dark-field hyperspectral X-ray imaging , 2014, Proceedings of the Royal Society A: Mathematical, Physical and Engineering Sciences.

[33]  Birgit Kanngießer,et al.  A new 3D micro X-ray fluorescence analysis set-up - First archaeometric applications , 2003 .