Many areas of material science have been transformed by the use of synchrotron radiation X-rays, including the fields of cultural heritage materials and biomineralization. This book presents a selection of contributions that illustrate recent developments and applications of these tools, focused either on the main techniques used in the cultural heritage and biomineralization communities or on specific materials, studying their intrinsic properties or how they change with time.
Each chapter can be read alone, and each individually demonstrates the intimate links between materials and methods. The chapters explore the main principles of synchrotron radiation, as well as techniques based on X-ray absorption and diffraction, and give an overview of how these approaches have developed in recent decades in the field of cultural heritage, with specific examples such as ancient ceramics, corrosion of iron-based materials, concrete used in Roman monuments and the biomineralization process in sea urchin spines.
Table of Content
Preface
Catherine Dejoie, Pauline Martinetto And Nobumichi Tamura
Chapter 1 Introduction to Synchrotron Radiation: Application to the Study of Cultural Heritage Materials and Biominerals 1
Catherine Dejoie, Pauline Martinetto And Nobumichi Tamura
1.1 Introduction 1
1.2 What is synchrotron radiation? 3
1.3 Synchrotron radiation and Cultural Heritage 8
1.4 Conclusion 11
1.5 Acknowledgments 12
1.6 References 12
Chapter 2 Development of the Use of Synchrotron Radiation for the Study of Cultural Heritage Materials 17
Nobumichi Tamura, Catherine Dejoie And Pauline Martinetto
2.1 Introduction 17
2.2 Synchrotron techniques used in the study of cultural heritage materials 21
2.3 Study of specific pigments in ceramics, sculptures and murals 24
2.3.1 Iron oxide pigments in Jian wares 25
2.3.2 Maya Blue pigment in Mesoamerica 27
2.4 Study of paintings 32
2.5 Study of murals and rock art 35
2.6 Study of cosmetics 37
2.7 Study of parchments and manuscripts 38
2.8 Artwork restoration and preservation effort with synchrotron 40
2.9 Other cultural heritage studies 43
2.10 Study in paleontology 45
2.11 Conclusion 49
2.12 Acknowledgments 50
2.13 References 50
Chapter 3 Application of Full-field X-ray Absorption Spectroscopy Imaging in Transmission Mode to Study Cultural Heritage Samples 69
Emeline Pouyet, Letizia Monico, Philippe Sciau And Marine Cotte
3.1 Introduction 70
3.2 The worldwide context of tender and hard X-ray domain FF-XANES instruments 73
3.3 Typical acquisition, processing and sample preparation strategies for CH studies: the example of the FF-XANES set-up at beamline ID21 (ESRF) 75
3.3.1 Sample preparation 75
3.3.2 Acquisition and data pre-processing 77
3.3.3 Data analysis workflow 78
3.3.4 A low fluence chemical imaging strategy for dedicated case studies 79
3.4 Applications of FF-XANES to study CH samples 82
3.4.1 Painting composition and degradation: historical cases and paint mock-ups 82
3.4.2 Combined instrumentation for a representative multi-scale characterization: the example of estimating firing conditions in ancient Roman ceramics 88
3.5 Conclusion 91
3.6 Acknowledgments 92
3.7 References 93
Chapter 4 Structural Cartography and Tomography by Diffraction/Diffusion: A Local Selective Analysis of Cultural Heritage Materials 101
Jean-Louis Hodeau, Michèle Alvarez-Murga, Michel Anne, Pierre-Olivier Autran, Nils Blanc, Pierre Bleuet, Nathalie Boudet, Pierre Bordet, Sophie Cersoy, Catherine Dejoie, Eric Dooryhée, Florian Kergoulay, Olivier Leynaud, Pauline Martinetto, Alain Prat And Philippe Walter
4.1 Introduction 102
4.2 2D mapping using diffraction 104
4.2.1 First imaging experiments 104
4.2.2 2D mapping of a “raw” heritage artifact 105
4.2.3 Complementarity of 2D mappings performed on samples and/or directly on artworks: the example of Lead White 110
4.3 3D mapping by tomography 115
4.3.1 Method history 115
4.3.2 3D tomography with different modes of physical interactions 116
4.3.3 Different types of 3D diffraction tomography 117
4.4 Diffraction/scattering computed tomography: DSCT 118
4.4.1 Initial DSCT experiments 118
4.4.2 Methodology of DSCT analyses and reconstructions 120
4.4.3 Selectivity of DSCT analyses 121
4.4.4 Selectivity of “multimodal” DSCT analyses 124
4.4.5 The wide range of DSCT applications 126
4.4.6 Analysis tools for DSCT imaging 127
4.4.7 DSCT analyses dedicated to heritage materials 128
4.5 Conclusion 133
4.6 Acknowledgments 134
4.7 References 134
Chapter 5 Contribution of Synchrotron Radiation to the Study of Glazed Ancient Ceramics 151
Philippe Sciau And Chantal Brouca-Cabarrecq
5.1 Introduction 151
5.2 The problem 152
5.3 Spectroscopic techniques 155
5.3.1 Microbeam absorption spectroscopy 155
5.3.2 “Full-field” imaging and spectroscopy 162
5.4 Diffraction techniques 168
5.4.1 With a monochromatic beam (powder diffraction) 168
5.4.2 With a polychromatic beam (Laue method) 171
5.5 Conclusion 177
5.6 References 178
Chapter 6 Relevant Synchrotron X-rays Techniques to Study Corroded Iron Cultural Heritage Material 181
Solenn Réguer, François Mirambet, Judith Monnier, Delphine Neff, Eddy Foy And Philippe Dillmann
6.1 Introduction 181
6.2 Iron corrosion diagnosis in historical monuments 185
6.2.1 Identification of the corrosion products 185
6.2.2 Specific chemical elements from the elaboration processes 187
6.3 In situ experiments for a direct observation of corrosion processes 190
6.3.1 How to reveal atmospheric corrosion processes? 190
6.3.2 Iron corrosion in cement matrices of ancient building 191
6.4 Archaeological objects corrosion and stabilization 192
6.4.1 Corrosion in anoxic soils 192
6.4.2 Specific Cl-containing corrosion products 193
6.4.3 Dechlorination treatment revealed 195
6.5 Protection of ancient iron artifacts 195
6.6 Conclusion and outlook 196
6.7 Acknowledgments 197
6.8 References 198
Chapter 7 Synchrotron X-Ray Microdiffraction Studies of the Mortars of Ancient Roman Concretes 203
Marie D. Jackson, Heng Chen, Jacob G. Peterson, Cagla Meral Akgul And Bryony Richards
7.1 Introduction 203
7.2 Standard powder X-ray diffraction studies of Roman mortars 206
7.3 Synchrotron µXRD and µXRF studies of ancient Roman mortars 210
7.4 Architectural mortars – Markets and Forum of Trajan 212
7.4.1 Cementing matrix 213
7.4.2 Vesicular scoria 215
7.4.3 Pumiceous aggregate 215
7.5 Marine harbor mortar – Baianus Sinus Bay of Pozzuoli 216
7.5.1 Relict lime clast and cementing matrix 219
7.5.2 Relict spherical void 220
7.6 Roman principles of concrete longevity 222
7.7 Conclusion 224
7.8 Acknowledgments 224
7.9 References 224
Chapter 8 Biomineralization in Sea Urchin Spines: A View on Amorphous Calcium Carbonate Occurrence, Stabilization and Crystallization 233
Marie Albéric And Ronald Seidel
8.1 Introduction 233
8.2 Biomineralization in sea urchins 235
8.3 Occurrence of ACC precursors in regenerated sea urchin spines 239
8.3.1 Why X-ray photoemission electron spectromicroscopy and how? 239
8.3.2 Ca L 2, 3-edge XANES spectra 240
8.3.3 Calcium component maps 241
8.4 ACC structure and stability: role of water and ion impurities 242
8.4.1 ACCs structure 242
8.4.2 Why pair distribution function analysis and how? 243
8.4.3 PDFs of ACC and Mg-ACC 245
8.4.4 In situ PDFs during the crystallization of ACC and Mg-ACC 246
8.5 Induced crystallization of remnant ACC in sea urchin spines 247
8.5.1 Why high-resolution X-ray diffraction and how? 247
8.5.2 Biogenic calcite lattice distortions 250
8.5.3 Why in situ Small Angle X-ray Scattering and how? 251
8.5.4 Quantification of the nanoporosity 251
8.6 Conclusion 252
8.7 Acknowledgments 253
8.8 References 253
List of Authors 263
Index 267
About the author
Catherine Dejoie is Beamline Scientist at the European Synchrotron Radiation Facility, France, and specializes in synchrotron X-ray diffraction techniques and their application in the fields of microporous materials and cultural heritage materials.
Pauline Martinetto is Assistant Professor at the University Grenoble-Alpes, France. She primarily works on the development of X-ray based techniques in the field of cultural heritage materials.
Nobumichi Tamura is Senior Scientist at the Advanced Light Source of the Lawrence Berkeley National Lab, USA, and specializes in synchrotron X-ray techniques, with a special interest in archeology, biomineralization and paleontology.
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