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Fifth volume of a 40 volume series on nanoscience and nanotechnology, edited by the renowned scientist Challa S.S.R. Kumar. This handbook gives a comprehensive overview about X-ray and Neutron Techniques for Nanomaterials Characterization. Modern applications and state-of-the-art techniques are covered and make this volume an essential reading for research scientists in academia and industry.



1. Synchrotron X-Ray Phase Nanotomography for Bone Tissue Characterization

X-ray phase nano-tomography allows the characterisation of bone ultrastructure: the lacuno-canalicular network, nanoscale mineralisation and the collagen orientation. In this chapter, we review the different X-ray imaging techniques capable of imaging the bone ultrastructure and then describe the work that has been done so far in nanoscale bone tissue characterisation using X-ray phase nano-tomography.X-ray computed tomography at the micrometric scale is more and more considered as the reference technique in imaging of bone microstructure. The trend has been to push towards higher and higher resolution. Due to the difficulty of realising optics in the hard X-ray regime, the magnification has mainly been due to the use of visible light optics and indirect detection of the X-rays, which limits the attainable resolution with respect to the wavelength of the visible light used in detection. Recent developments in X-ray optics and instrumentation have allowed the implementation of several types of methods that achieve imaging limited in resolution by the X-ray wavelength, thus enabling computed tomography at the nanoscale. We review here the X-ray techniques with 3D imaging capability at the nanoscale: transmission X-ray microscopy, ptychography and in-line holography. Then, we present the experimental methodology for the in-line phase tomography, both at the instrumentation level and the physics behind this imaging technique. Further, we review the different ultrastructural features of bone that have so far been resolved and the applications that have been reported: imaging of the lacuno-canalicular network, direct analysis of collagen orientation, analysis of mineralisation on the nanoscale and the use of 3D images at the nanoscale as the basis of mechanical analyses. Finally, we discuss the issue of going beyond qualitative description to quantification of ultrastructural features.

Peter Varga, Loriane Weber, Bernhard Hesse, Max Langer

2. 3D Chemical Imaging of Nanoscale Biological, Environmental, and Synthetic Materials by Soft X-Ray STXM Spectrotomography

Gregor Schmid, Martin Obst, Juan Wu, Adam Hitchcock

3. X-Ray Photon Correlation Spectroscopy for the Characterization of Soft and Hard Condensed Matter

Oier Bikondoa

4. XAFS for Characterization of Nanomaterials

X-ray absorption fine structure (XAFS) spectroscopy studies the modification of the X-ray absorption coefficient, above the absorption edge of a specific element, due to the presence of neighboring atoms and delivers information on materials nano- and electronic structure. The long-range translational symmetry is not a prerequisite, as in the case of diffraction-based techniques, which, along with the atom-specific character of XAFS, renders it a powerful tool for the study of nanomaterials.In the following the principles of XAFS spectroscopy will be discussed. A brief introduction of the theoretical basis of the spectroscopy will be presented, the emphasis being on the phenomena that affect the spectrum at energies below, near, and far above the absorption edge. In addition to that, the main experimental setups used for the acquisition of the XAFS spectra in the soft and hard X-ray regimes will also be presented. Furthermore, the analysis procedure of the extended part of the XAFS (called extended XAFS, acronym EXAFS) spectrum and the related parameters, as well as methodologies followed in the analyses of the near-edge part of the spectrum (called X-ray absorption near-edge structure or near-edge X-ray absorption fine structure, the corresponding acronyms being XANES and NEXAFS, respectively), will be described. Finally, recently published representative applications of XAFS spectroscopy for the study of various types of nanomaterials, for example, nanocatalysts, carbon-based nanomaterials, semiconductor quantum dots, etc., will be reviewed.

Maria Katsikini, Eleni C. Paloura

5. The Characterization of Atomically Precise Nanoclusters Using X-Ray Absorption Spectroscopy

The XAS toolbox (EXAFS, XANES, theoretical calculations, in situ measurements) is used in a variety of applications to determine the structure and electronic properties of atomically precise nanoclusters (APNCs). The analysis using the EXAFS part of the XAS spectrum involves models that are based on atomic packing (e.g., fcc, icosahedra) or surface effects. Theoretical methods based on DFT can improve the understanding of disorder effects on the EXAFS measurements. In comparative experiments, the effect of solvation and of the ligands (density of ligands, different ligands) is discussed. It was found that the strength of the Au–thiol bonding can lead to relaxation effects that reduce the contraction of Au–Au bonds in the core. Changes in structure could be observed for solvation and catalytic reaction with the application of in situ measurements in specifically designed reactors. Even though EXAFS is a powerful method with a number of advantages, such as that no long-range order is necessary, all kinds of materials can be investigated, nondestructively. The analysis of EXAFS data is quite challenging, however, and effects such as structural disorder, if the sample is a mixture of components (not pure) or if the APNCs have several binding ligands, can distort the results. The use of l-DOS based on theoretical XANES calculations that can give information about electronic properties of APNCs is also challenging. In complement with XPS experiments, however, consistent answers can be found.

Lisa Bovenkamp-Langlois, Martha W. Schaefer

6. X-Ray Absorption Spectroscopic Characterization of Nanomaterial Catalysts in Electrochemistry and Fuel Cells

Kotaro Sasaki, Nebojsa Marinkovic

7. In Situ SXS and XAFS Measurements of Electrochemical Interface

In this chapter, we focus on structural studies at electrode/electrolyte solution interfaces by means of surface x-ray scattering (SXS) and x-ray absorption fine structure (XAFS) measurements using synchrotron radiation (SR) light as an x-ray source. After describing the importance of these techniques for structural studies at the electrode/electrolyte interface as an introduction, we explain the fundamental principles and experimental methodologies of these techniques. Finally, we describe trends in the development of these techniques and review the latest topics.

Toshihiro Kondo, Takuya Masuda, Kohei Uosaki

8. Gas-Phase Near-Edge X-Ray Absorption Fine Structure (NEXAFS) Spectroscopy of Nanoparticles, Biopolymers, and Ionic Species

Near-edge X-ray absorption fine structure (NEXAFS) spectroscopy probes directly or indirectly the photoabsorption cross section of a system under study as a function of the photon energy around the core–shell ionization thresholds. When the photon energy matches the difference between the core level and an unoccupied valence level, the photoabsorption cross section increases. The core levels are associated with particular atoms within the system under the study; therefore, NEXAFS spectroscopy appears to be a very sensitive probe of physicochemical and structural properties of molecules and materials. It has been intensively applied to investigate gaseous, liquid, and solid species. In this chapter, we describe methods to perform gas-phase NEXAFS spectroscopy of large systems, such as nanoparticles, clusters, and biopolymers, as well as of ionic species. We also review recent research findings.The development of third-generation synchrotron radiation (SR) sources, providing extremely bright and energy-resolved X-ray beams, established NEXAFS spectroscopy as a powerful and widely used technique to investigate electronic and structural properties of both organic and inorganic samples of increasing complexity. Particularly, gas-phase NEXAFS studies allow for an investigation of well-defined targets prepared under desired conditions.Unfortunately, gas-phase NEXAFS spectroscopy of large species such as biopolymers (e.g., proteins and DNA) and nanoparticles, as well as ionic species, is experimentally very challenging due to great difficulties in both bringing large molecules or particles intact into the gas phase and providing high-enough target density, photon flux, and interaction time needed to distinguish K-shell excitation processes. Only recently, the development of new experimental techniques has allowed performing gas-phase NEXAFS of nanoparticles, biopolymers, and ionic species.Herein, we present the basic principles of NEXAFS spectroscopy and describe the state-of-the-art experimental approaches that allow for NEXAFS spectroscopy of large biopolymers and nanoparticles isolated in the gas phase. Finally, we present some key research finding spanning from relatively small biomolecules to large biopolymers and nanoparticles.

Aleksandar R. Milosavljević, Alexandre Giuliani, Christophe Nicolas

9. In Situ X-Ray Reciprocal Space Mapping for Characterization of Nanomaterials

Peter Siffalovic, Karol Vegso, Martin Hodas, Matej Jergel, Yuriy Halahovets, Marco Pelletta, Dusan Korytar, Zdeno Zaprazny, Eva Majkova

10. X-Ray Powder Diffraction Characterization of Nanomaterials

We discuss here what important knowledge can be gained by X-ray diffraction (of course, more specifically, we talk of X-ray powder diffraction) experiments on nanoparticles and nanomaterials in general. Historically, the uses of X-ray diffraction have been to investigate (a) the crystal structure of materials at the atomic scale and (b) their microstructure, a broad term meaning deviations from perfect crystalline order on a scale that is larger than the atomic one but still microscopic. In fact, macroscopic properties of materials tend to depend on both of those. For nanomaterials, the focus is to understand how the small crystal domain extension and related phenomena influence properties that differ – often in a very useful way – from the parent crystalline material. This means that the focus is on the microstructure, due to the fact that reduced domain extension is a (strong) deviation from crystal order – this is by definition something that extends to infinity. Of course there exist crystalline phases that are stable only at the nanoscale – and in such case, the crystal structure determination still is very important. In this contribution, we shall review all modern experimental methods and especially – as this is the core of the method – the data analysis techniques currently used, from the oldest, based on the Bragg formalism to interpret crystal diffraction, to the newest, relying on atomic-scale modeling.

Antonio Cervellino, Ruggero Frison, Norberto Masciocchi, Antonietta Guagliardi

11. X-Ray Absorption Fine Structure Analysis of Catalytic Nanomaterials

Wang-Jae Chun, Satoru Takakusagi, Yohei Uemura, Kyoko Bando, Kiyotaka Asakura

12. Contribution of Small-Angle X-Ray and Neutron Scattering (SAXS and SANS) to the Characterization of Natural Nanomaterials

Small-angle neutron scattering (SANS) and small-angle X-ray scattering (SAXS) are well-established techniques that have been successfully used in nanoscale structure determination of synthetic or manufactured systems used in soft matter or materials domain. In this chapter, we examine the application of such techniques to determine features of natural nano-materials encountered in the petroleum and new energy industry.Successful implementation of industrial processes depends partly on understanding of systems in use conditions. Hence, for transformation of natural materials, a good knowledge of structure and behavior of these materials in process conditions is desirable. Among natural materials, few of them are nanostructured, and very few techniques are available to characterize these systems in thermodynamic and hydrodynamic conditions close to one encountered in the industrial process.Small-angle scattering (SAS) techniques, either X-ray or neutrons, has the potential, but its use is sometimes limited to manufactured or synthetic systems. Laboratory SAXS equipments become more popular but remain sparse, especially in industrial environment. Large-scale facilities such as synchrotron or neutron centers have been used for academic research but open now more and more to industrial issues. The aim of this chapter is to discuss the contribution of SAXS and SANS to the characterization of natural nano-materials.Two different nanostructured materials will be examined here. The first one comes from heavy cuts of petroleum where the largest and most aromatic molecules – the asphaltenes – self-associate. The behavior of such aggregates generally impairs processes. This aggregation behavior will be examined in the bulk as well as at liquid/liquid or liquid/solid interfaces. A special attention will be paid to observation close to use conditions. The second ones are geomaterials, including sedimentary rocks and gas and oil shales. For these materials, the pore size distribution (open versus closed porosity, accessibility of pores to various fluids) is of primary interest leading to a better understanding of gas storage and transport mechanisms and their controls.We will show, through the study of these two nanostructured materials, how SAS techniques contribute to the characterization of such systems.

Loïc Barré

13. Synchrotron Small-Angle X-Ray Scattering and Small-Angle Neutron Scattering Studies of Nanomaterials

Hiroyuki Takeno

14. Quasielastic Neutron Scattering: An Advanced Technique for Studying the Relaxation Processes in Condensed Matter

Madhusudan Tyagi, Suresh M. Chathoth


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