Three Dimensional X Ray Diffraction Microscopy

Three-dimensional x-ray diffraction (3DXRD) microscopy is a novel experimental method for structural characterisation of polycrystalline materials. The position, morphology, phase, strain and crystallographic orientation of hundreds of grains or sub-grain embedded within mm-cm thick specimens can be determined simultaneously. Furthermore, the dynamics of the individual structural elements can be monitored during typical processes such as deformation or annealing. The book gives a comprehensive account of the methodology followed by a summary of selected applications. The method is presented from a mathematical/crystallographic point-of-view but with sufficient hands-on details to enable the reader to plan his or her own experiments. The scope of applications includes work in materials science and engineering, geophysics, geology, chemistry and pharmaceutical science.

The ability to interpret and inverse x-ray diffraction patterns from crystals has largely shaped our understanding of the structure of matter. However, structure determination of noncrystalline objects from their diffraction patterns is a much more difficult task. The dramatic increase in available coherent x-ray photon flux over the past decade has made possible a technique known as lensless coherent diffractive imaging (CDI), that addresses exactly this problem. The central question around CDI is the so-called phase problem: upon detection of the diffraction intensity, the phase information of the diffracted wave is inevitably lost. Generally, the phase problem is approached using iterative phase retrieval algorithms. Holographic methods, through interference with reference diffractions, encode the phase information directly inside the measured x-ray holograms, and are therefore able to avoid the stagnation and uniqueness problems commonly encountered by the iterative algorithms. This dissertation discusses two novel holographic methods for coherent lensless imaging using resonant soft x-rays. The first part focuses on generalizing the multiple-wavelength anomalous diffraction technique, a highly successful method for solving the crystal structures of biomacromolecules, into a multiple-wavelength holography technique for nanoscale resonant x-ray imaging. Using this method I show element specific reconstructions of nanoparticles and magnetization distribution in magnetic thin films with sub 50 nm resolution. The second part discusses progress in X-ray Fourier holography, an ultrafast lensless imaging platform that can be used with the upcoming x-ray free electron lasers. In particular, I will present experiments using two novel types of extended reference structures that bring the resolution beyond the precision of reference fabrication, previously regarded as the resolution limit for x-ray Fourier transform holography. Finally, future applications of holographic methods, especially experimental considerations for time-resolved studies of nanostructures using X-FELs, will be discussed.

Authored by a university professor deeply involved in X-ray diffraction-related research, this textbook is based on his lectures given to graduate students for more than 20 years. It adopts a well-balanced approach, describing basic concepts and experimental techniques, which make X-ray diffraction an unsurpassed method for studying the structure of materials. Both dynamical and kinematic X-ray diffraction is considered from a unified viewpoint, in which the dynamical diffraction in single-scattering approximation serves as a bridge between these two parts. The text emphasizes the fundamental laws that govern the interaction of X-rays with matter, but also covers in detail classical and modern applications, e.g., line broadening, texture and strain/stress analyses, X-ray mapping in reciprocal space, high-resolution X-ray diffraction in the spatial and wave vector domains, X-ray focusing, inelastic and time-resolved X-ray scattering. This unique scope, in combination with otherwise hard-to-find information on analytic expressions for simulating X-ray diffraction profiles in thin-film heterostructures, X-ray interaction with phonons, coherent scattering of Mossbauer radiation, and energy-variable X-ray diffraction, makes the book indispensable for any serious user of X-ray diffraction techniques. Compact and self-contained, this textbook is suitable for students taking X-ray diffraction courses towards specialization in materials science, physics, chemistry, or biology. Numerous clear-cut illustrations, an easy-to-read style of writing, as well as rather short, easily digestible chapters all facilitate comprehension.

This book addresses the current status, challenges and future directions of data-driven materials discovery and design. It presents the analysis and learning from data as a key theme in many science and cyber related applications. The challenging open questions as well as future directions in the application of data science to materials problems are sketched. Computational and experimental facilities today generate vast amounts of data at an unprecedented rate. The book gives guidance to discover new knowledge that enables materials innovation to address grand challenges in energy, environment and security, the clearer link needed between the data from these facilities and the theory and underlying science. The role of inference and optimization methods in distilling the data and constraining predictions using insights and results from theory is key to achieving the desired goals of real time analysis and feedback. Thus, the importance of this book lies in emphasizing that the full value of knowledge driven discovery using data can only be realized by integrating statistical and information sciences with materials science, which is increasingly dependent on high throughput and large scale computational and experimental data gathering efforts. This is especially the case as we enter a new era of big data in materials science with the planning of future experimental facilities such as the Linac Coherent Light Source at Stanford (LCLS-II), the European X-ray Free Electron Laser (EXFEL) and MaRIE (Matter Radiation in Extremes), the signature concept facility from Los Alamos National Laboratory. These facilities are expected to generate hundreds of terabytes to several petabytes of in situ spatially and temporally resolved data per sample. The questions that then arise include how we can learn from the data to accelerate the processing and analysis of reconstructed microstructure, rapidly map spatially resolved properties from high throughput data, devise diagnostics for pattern detection, and guide experiments towards desired targeted properties. The authors are an interdisciplinary group of leading experts who bring the excitement of the nascent and rapidly emerging field of materials informatics to the reader.

Cryoelectron microscopy of biological molecules is among the hottest growth areas in biophysics and structural biology at present, and Frank is arguably the most distinguished practitioner of this art. CryoEM is likely over the next few years to take over much of the structural approaches currently requiring X-ray crystallography, because one can now get good and finely detailed images of single molecules down to as little as 200,000 MW, covering a substantial share of the molecules of greatest biomedical research interest. This book, the successor to an earlier work published in 1996 with Academic Press, is a natural companion work to our forthcoming book on electron crystallography by Robert Glaeser, with contributions by six others, including Frank. A growing number of workers will employ CryoEM for structural studies in their own research, and a large proportion of biomedical researchers will have a growing interest in understanding what the capabilities and limits of this approach are.

An indispensable resource for researchers and students in materials science, chemistry, physics, and pharmaceuticals Written by one of the pioneers of 2D X-Ray Diffraction, this updated and expanded edition of the definitive text in the field provides comprehensive coverage of the fundamentals of that analytical method, as well as state-of-the art experimental methods and applications. Geometry convention, x-ray source and optics, two-dimensional detectors, diffraction data interpretation, and configurations for various applications, such as phase identification, texture, stress, microstructure analysis, crystallinity, thin film analysis, and combinatorial screening are all covered in detail. Numerous experimental examples in materials research, manufacture, and pharmaceuticals are provided throughout. Two-dimensional x-ray diffraction is the ideal, non-destructive analytical method for examining samples of all kinds including metals, polymers, ceramics, semiconductors, thin films, coatings, paints, biomaterials, composites, and more. Two-Dimensional X-Ray Diffraction, Second Edition is an up-to-date resource for understanding how the latest 2D detectors are integrated into diffractometers, how to get the best data using the 2D detector for diffraction, and how to interpret this data. All those desirous of setting up a 2D diffraction in their own laboratories will find the author’s coverage of the physical principles, projection geometry, and mathematical derivations extremely helpful. Features new contents in all chapters with most figures in full color to reveal more details in illustrations and diffraction patterns Covers the recent advances in detector technology and 2D data collection strategies that have led to dramatic increases in the use of two-dimensional detectors for x-ray diffraction Provides in-depth coverage of new innovations in x-ray sources, optics, system configurations, applications and data evaluation algorithms Contains new methods and experimental examples in stress, texture, crystal size, crystal orientation and thin film analysis Two-Dimensional X-Ray Diffraction, Second Edition is an important working resource for industrial and academic researchers and developers in materials science, chemistry, physics, pharmaceuticals, and all those who use x-ray diffraction as a characterization method. Users of all levels, instrument technicians and X-ray laboratory managers, as well as instrument developers, will want to have it on hand.

This book provides a detailed, self-contained description of automatic indexing of crystal diffraction patterns, considering both ab initio indexing and indexing of patterns originating from known structures. Introductory chapters equip the reader with the necessary basic knowledge of geometric crystallography, as well as kinematic and dynamic theories of crystal diffraction. Subsequent chapters delve and describe ab initio indexing of single crystal diffraction patterns and indexing of patterns for orientation determination. The book also reviews methods of indexing powder diffraction and electron spot-type patterns, as well the subject of multigrain indexing. Later chapters are devoted to diffraction by helical structures and quasicrystals, as well as some aspects of lattice parameter refinement and strain determination. The book is intended equally for materials scientists curious about ‘nuts and bolts’ of diffraction pattern indexing and orientation mapping systems, as well as interdisciplinary researchers from physics, chemistry, and biology involved in crystallographic computing. It provides a rigorous, yet accessible, treatment of the subject matter for graduate students interested in understanding the functioning of diffraction pattern indexing engines.