X-Rays and Materials E-Book

• Herausgeber: John Wiley & Sons
• Kategorie: Fachliteratur
• Sprache: Englisch

Seitenzahl: 232

Veröffentlichungsjahr: 2013

Beschreibung

This book presents reviews of various aspects of radiation/matter interactions, be these instrumental developments, the application of the study of the interaction of X-rays and materials to a particular scientific field, or specific methodological approaches.

The overall aim of the book is to provide reference summaries for a range of specific subject areas within a pedagogical framework. Each chapter is written by an author who is well known within their field and who has delivered an invited lecture on their subject area as part of the "RX2009 – X-rays and Materials" colloquium that took place in December 2009 at Orsay in France.

The book consists of five chapters on the subject of X-ray diffraction, scattering and absorption:

• Chapter 1 gives a detailed presentation of the capabilities and potential of beam lines dedicated to condensed matter studies at the SOLEIL synchrotron radiation source.
• Chapter 2 focuses on the study of nanoparticles using small-angle X-ray scattering.
• Chapter 3 discusses the quantitative studies of this scattering signal used to analyze these characteristics in detail.
• Chapter 4 discusses relaxor materials, which are ceramics with a particularly complex microstructure.
• Chapter 5 discusses an approach enabling the in situ analysis of these phase transitions and their associated microstructural changes.

Leseprobe

Table of Contents

Preface

Chapter 1: Synchrotron Radiation: Instrumentation in Condensed Matter

1.1. Introduction

1.2. Light sources in the storage ring

1.3. Emittance and brilliance of a source

1.4. X-ray diffraction with synchrotron radiation

1.5. X-ray absorption spectroscopy using synchrotron radiation

1.6. SAMBA: the X-ray absorption spectroscopy beam line of SOLEIL for 4–40 keV

1.7. The DIFFABS beam line

1.8. CRISTAL beam line

1.9. The SOLEIL ODE line for dispersive EXAFS

1.10. Conclusion

1.11. Bibliography

Chapter 2: Nanoparticle Characterization using Central X-ray Diffraction

2.1. Introduction

2.2. Definition of scattered intensity

2.3. Invariance principle

2.4. Behavior for large q: the Porod regime

2.5. Particle-based systems

2.6. An absolute scale for measuring particle numbers

2.7. Conclusion

2.8. Bibliography

Chapter 3: X-ray Diffraction for Structural Studies of Carbon Nanotubes and their Insertion Compounds

3.1. Introduction

3.2. Single-walled carbon nanotubes

3.3. Multi-walled carbon nanotubes

3.4. Hybrid nanotubes

3.5. Textured powder samples

3.6. Conclusion

3.7. Bibliography

Chapter 4: Dielectric Relaxation and Morphotropic Phases in Nanomaterials

4.1. Introduction

4.2. Dielectric relaxation and morphotropic region: definition and mechanism

4.3. Relaxation, morphotropic region and size reduction

4.4. Conclusion

4.5. Acknowledgements

4.6. Bibliography

Chapter 5: Evolution of Solid-state Microstructures in Polycrystalline Materials: Application of High-energy X-ray Diffraction to Kinetic and Phase Evolution Studies

5.1. Introduction

5.2. Experimental methods

5.3. Results

5.4. Conclusion

5.5. Acknowledgements

5.6. Bibliography

List of Authors

Index

First published 2012 in Great Britain and the United States by ISTE Ltd and John Wiley & Sons, Inc.

Apart from any fair dealing for the purposes of research or private study, or criticism or review, as permitted under the Copyright, Designs and Patents Act 1988, this publication may only be reproduced, stored or transmitted, in any form or by any means, with the prior permission in writing of the publishers, or in the case of reprographic reproduction in accordance with the terms and licenses issued by the CLA. Enquiries concerning reproduction outside these terms should be sent to the publishers at the undermentioned address:

ISTE Ltd 27-37 St London SW19 4EU UKwww.iste.co.ukJohn Wiley & Sons, Inc. George’s Road 111 River Street Hoboken, NJ 07030 USAwww.wiley.com

© ISTE Ltd 2012

The rights of Philippe Goudeau and René Guinebretière to be identified as the author of this work have been asserted by them in accordance with the Copyright, Designs and Patents Act 1988.

Library of Congress Cataloging-in-Publication Data

X-rays and materials / edited by Philippe Goudeau, René Guinebretière. p. cm.

Includes bibliographical references and index.

ISBN 978-1-84821-342-5 (hardback)

1. Materials--Analysis. 2. X-ray microanalysis. 3. X-rays--Diffraction. 4. X-ray spectroscopy. I. Goudeau, Philippe. II. Guinebretière, René.

TA417.25.X758 2012 620.1'1272--dc23

British Library Cataloguing-in-Publication Data A CIP record for this book is available from the British Library ISBN: 978-1-84821-342-5

Preface1

This book presents reviews of various aspects of radiation/matter interactions, be these instrumental developments, the application of the study of the interaction of X-rays and materials to a particular scientific field, or specific methodological approaches. The overall aim of the book is to provide reference summaries for a range of specific subject areas within a pedagogical framework. Each chapter is written by an author who is well known within their field and who has delivered an invited lecture on their subject area as part of the “RX2009 – X-rays and Materials” colloquium that took place in December 2009 at Orsay.

For some years now, a new tool has been available in France for the exploration of the properties of materials through the use of X-rays. This is the SOLEIL synchrotron radiation source, which is now fully operational. It is able to respond to an ever-growing demand for “beam time”. It is also able to push the boundaries of certain areas of materials science. Our intention was that this book should be strongly focused on the use of synchrotron radiation.

This book consists of five chapters on the subject of X-ray diffraction, scattering and absorption.

Chapter 1 gives a detailed presentation of the capabilities and potential of beam lines dedicated to condensed matter studies at the SOLEIL synchrotron radiation source. After a general discussion of the source itself and the techniques involved, the authors of this chapter give a detailed discussion of the configurations that are available and the applications that have been developed around the “SAMBA”, “DIFFABS”, “CRISTAL” and “ODE” beam lines. Throughout this chapter, particular attention is paid to the discussion of how the different techniques can complement each other, as well as the development of apparatus for measurement under thermal stress or high pressure.

When the objects interacting with the X-rays are nanometer-sized in addition to the diffraction signal that would be observed when they are crystallized, there is also a significant scattering contribution that appears around the center of the reciprocal lattice. This is referred to as “central X-ray scattering”, or more commonly as “small-angle scattering”. The pioneering work carried out by André Guinier has put the French scientific community in a strong position in this field. Bizarrely, few recent reviews pay much attention to this technique.

Chapter 2 focuses on the study of nanoparticles using small-angle X-ray scattering. It discusses in detail the formalism that can be used to interpret the scattering signal in terms of the size and shape of the particles that generate it. Extrapolation of the signal to the center of the reciprocal lattice space makes it possible to determine the volume of scattering material, and the author illustrates the potential of this technique with in situ monitoring of the seeding of gold nanoparticles.

Imperfections within the crystal lead to the appearance of localized “diffuse scattering”, which this time is not at the center of the reciprocal lattice but around the Bragg peaks. Since the discovery of carbon nanotubes around the start of the 1990s, their study has attracted a huge scientific community of chemists, biologists and condensed matter physicists. X-ray scattering is an ideal technique for performing quantitative measurements of the structural characteristics of carbon nanotubes: diameter, number of walls, lattice orientation, as well as examining the integration of fullerenes inside the tubes. Chapter 3 discusses the quantitative studies of this scattering signal used to analyze these characteristics in detail.

Chapter 4 discusses relaxor materials, which are ceramics with a particularly complex microstructure. These materials, with a paraelectric-ferroelectric transition temperature that is a function of the frequency of the applied electric field, consist of nanometer-sized regions with a different polarization to that of the matrix surrounding them. These are often associated with chemical inhomogeneities and local deformations of the crystal lattice. Here again, as in the previous chapter, diffuse scattering is observed around the Bragg peaks, and this provides information on these very specific microstructural characteristics.

The author of Chapter 4 is the head of a laboratory that has been heavily involved in this field for more than 20 years. He presents an in-depth discussion of this application area of X-ray diffraction and scattering. The reader will discover that the interpretation of this signal remains a highly controversial subject, but also that X-ray scattering is pivotal to the study of the nanometer-scale microstructure of these types of material.

The fabrication process for complex materials often includes thermal cycling, especially in metallurgy. The phase transitions that occur during these thermal treatments induce the appearance of specific microstructures that have a strong influence on the ultimate physical properties of the material. Chapter 5 discusses an approach enabling the in situ analysis of these phase transitions and their associated microstructural changes. Thus, the authors use a synchrotron to examine samples placed inside an oven, monitoring and quantifying the changes in the material using high-energy X-ray scattering. These measurements of the changes in lattice parameters and levels of transformed phases are performed with the help of a two-dimensional detector and, as a result, the acquisition times for the diagrams are in the order of a second, making it possible to observe the transformations occurring in real time.

1 Preface written by René GUINEBRETIÈRE and Philippe GOUDEAU.

Chapter 1

Synchrotron Radiation: Instrumentation in Condensed Matter1

1.1. Introduction

Since the appearance of third-generation sources, the use of synchrotron radiation has seen a significant growth over a wide range of disciplines (biology, chemistry, physics, environmental science, earth science, cultural studies, etc.). The reasons behind this success are the qualities of the beams that can be obtained (flux, brilliance, stability, etc.) and the development of optics that are able to exploit these qualities to their full potential. To this we can add the possibility of setting up a sophisticated environment around the sample, enabling it to be monitored in situ.

In this chapter we intend to describe the various types of source available in a synchrotron radiation facility and define their brilliance. We will see how the optics can be adapted to particular types of experiments (generally X-ray absorption and diffraction) in order to best preserve this brilliance. We will illustrate this by describing some of the beam lines from the SOLEIL synchrotron. We will also give examples of the sample environments installed on these beam lines (we will limit ourselves to the field of condensed matter).