Materials characterization by synchrotron x-ray microprobes and nanoprobes

Mino, Lorenzo; Borfecchia, Elisa; Segura-Ruíz, Jaime; Giannini, Cinzia; Martı́nez-Criado, Gema; Lamberti, Carlo

doi:10.1103/revmodphys.90.025007

Cited by 107 publications

(57 citation statements)

References 678 publications

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“…Employing SR‐based X‐ray microbeams/nanobeams, which is achievable through implementing proper optics and lenses, can provide us with invaluable information about microstructure and nanostructure in the depth of materials. Ice et al and Mino et al overviewed the most exquisite factors regarding the generation and recent developments of X‐ray microbeams/nanobeams.…”

Section: X‐ray Microbeam/nanobeammentioning

confidence: 99%

Review on applications of synchrotron‐based X‐ray techniques in materials characterization

2020

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Synchrotron radiation (SR), as a result of its high-intensity, brilliant, monochromatic, and collimated beams, is becoming one of the most crucial components of research in various fields of materials science such as nanomaterials, biomaterials, and energy materials. SR-based characterization methods can be employed to analyze different systems such as powders, thin films, and bulk forms having complex crystalline or amorphous structures. In this review, peculiarities of SR are briefly explained. Moreover, various techniques carried out utilizing this instrument for material characterization such as X-ray powder diffraction, grazing-incidence X-ray diffraction, small/ wide-angle X-ray scattering, X-ray absorption spectroscopy, different techniques of X-ray imaging, X-ray photoelectron spectroscopy, and X-ray microprobes/nanoprobes are presented. As a result, by shedding light on the advantages of SR and its superiority to the equivalent laboratory experiments, researchers are recommended to exploit the capabilities of this invaluable tool in their materials characterization.

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Section: X‐ray Microbeam/nanobeammentioning

confidence: 99%

Review on applications of synchrotron‐based X‐ray techniques in materials characterization

2020

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“…This approach is widely established in thermal catalysis (Newton and van Beek, 2010 ; O'Brien et al, 2011 ; Beale et al, 2013 , 2014 ; Liu et al, 2015 ) and is rapidly emerging in photocatalysis (Bora et al, 2013 , 2014 ; Dong and Vayssieres, 2018 ; Tan et al, 2019 ). A review on dedicated synchrotron X-ray microprobes and nanoprobes for in situ / operando material characterization has been reported recently (Mino et al, 2018 ).…”

Section: Qualitative Approaches For the Assessment Of Photocatalytic mentioning

confidence: 99%

Qualitative Approaches Towards Useful Photocatalytic Materials

Quesada-Cabrera

Parkin

2020

Front. Chem.

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The long-standing crusade searching for efficient photocatalytic materials has resulted in a vast landscape of promising photocatalysts, as reflected by the number of reviews reported in the last decade. Virtually all of these reviews have focused on quantitative approaches aiming at developing an understanding of the underlying mechanisms behind photocatalytic behavior and the parameters that influence structure-function correlation. Less attention has been paid, however, to qualitative measures around the development and assessment of photocatalysts. These measures will contribute toward narrowing the range of potential photocatalytic materials for widespread applications. The current report provides a critical perspective over some of the main factors affecting the assessment of photocatalytic materials as a code of good practice. A case of study is also provided, where this qualitative analysis is applied to one of the most prolific materials of the last-decade, disorder-engineered, black titanium dioxide (TiO 2).

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“…Working directly at the beamline is highly desirable for the end users in order to check during the experiment the quality of the acquired data and avoid undesirable loss of beamtime. This requirement is becoming of utmost importance considering the increase in the flux/brilliance of the new-generation sources and the reduction in the acquisition time granted by the new detectors (Mino et al, 2018). Let us suppose that in situ X-ray diffraction experiments in the PDF setup have been executed on one of the perovskite samples and that XRPD profiles have been continuously acquired with temperature.…”

Section: Model-independent Versus Model-dependent Analysesmentioning

confidence: 99%

Investigating temperature-induced structural changes of lead halide perovskites by in situ X-ray powder diffraction

et al. 2019

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In situ X‐ray diffraction experiments offer a unique opportunity to investigate structural dynamics at atomic resolution, by collecting several patterns in an appropriate time sequence (data matrix) while varying the applied stimulus (e.g. temperature changes). Individual measurements can be processed independently by refinement procedures that are based on prior knowledge of the average structure of each crystal phase present in the sample. If the refinement converges, parameters of the average structural model can be assessed and studied as a function of the stimulus variations. An alternative approach consists in applying a multivariate analysis to the data matrix as a whole. Methods such as principal component analysis (PCA) and phase‐sensitive detection perform fast, blind and model‐independent calculations that can be used for on‐site analysis to identify trends in data actually related to the applied stimulus. Both classical and multivariate approaches are here applied to the in situ X‐ray diffraction pair distribution function (PDF) setup on two samples of the hybrid perovskite methylammonium (MA) lead iodide obtained by different synthetic routes, subjected to temperature variations. The PDF refinement allows assessing the occurrence of temperature‐induced rotations of the PbI6 octahedra and variations in the relative amount of MAPbI3 and intermediate PbI2–MAI–DMSO (dimethyl sulfoxide) crystal phases. A change in the orientation of the methylammonium molecule with temperature is also characterized. Results of the multivariate analysis tools, which include a newly introduced space‐dependent variant of PCA, are described, interpreted and validated against simulated data, and their specificity and relation to refinement results are highlighted. The interaction between nearby octahedra is identified as the driving force for the tetragonal‐to‐cubic phase transition, and three fundamental trends in data having different temperature behaviours are unveiled: (i) irreversible weight‐fraction variations of the MAPbI3 and PbI2–MAI–DMSO phases; (ii) reversible structural changes related to the MAPbI3 crystalline phase and its lattice distortion in the ab plane, having the same frequency as the temperature variations; (iii) reversible lattice distortion along the c axis, occurring at twice the frequency of the temperature changes.

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Materials characterization by synchrotron x-ray microprobes and nanoprobes

Cited by 107 publications

References 678 publications

Review on applications of synchrotron‐based X‐ray techniques in materials characterization

Review on applications of synchrotron‐based X‐ray techniques in materials characterization

Qualitative Approaches Towards Useful Photocatalytic Materials

Investigating temperature-induced structural changes of lead halide perovskites by in situ X-ray powder diffraction

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