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THÈSE
Pour obtenir le grade de
DOCTEUR DE L’UNIVERSITÉ DE GRENOBLE
Spécialité : Physique de la matière condensée et du
rayonnement
Arrêté ministériel : 7 août 2006


Présentée par
Fabio MASIELLO

Thèse dirigée par Jürgen HÄRTWIG et
codirigée par Carlo LAMBERTI

préparée au sein du European Synchrotron Radiation Facility
dans l'École Doctorale de Physique

Diffraction et imagerie aux rayons
X en utilisant un faisceau
cohérent: applications aux
optiques rayons X et aux cristaux
comportant des hétérogénéités
de phase.


Thèse soutenue publiquement le 13 mai 2011
devant le jury composé de :
Dr. José BARUCHEL
Chercheur ESRF, Président
Pr. Brian TANNER
Professeur à l’Université de Durham – UK, Rapporteur
Pr. Simon CONNELL
Professeur à l’Université de Johannesburg – ZA, Membre
Dr. Pierre BASTIE
Chercheur ILL, Membre
Pr. Carlo LAMBERTI
Professeur a l’Université de Torino – I, Membre
Dr. Jürgen HÄRTWIG
Chercheur ESRF, Membre iiTo my Bibi...Acknowledgements
Here I am, finally writing the acknowledgments of my thesis. The first
person I am deeply indebted to is my theses (both MSc and PhD) supervisor,
Jurgen¨ H¨ artwig. The fact that, even during the more stressful period, you
have been able to sustain me with the right words and a smile is priceless!
It has been a real pleasure to work with you during almost five years and
to travel in four different continents together. Danke sch¨ on Herr H¨ artwig.
Thanks to Prof. Simon Connell, with whom, after creating a nice profes-
sional relationship, I am also managing to create a great familiar one. What
I found impressive about Simon is the fact that, whatever you chat with
him about (could be nuclear physics, diamond synthesis, the rules of rugby,
how to prepare a perfect braai or fixing a broken car) he is always able
to engross you in an amazing way. I feel very lucky that I will be able to
continue to listen to you for many years to come! But one thing is sure, I
will never ever think that rugby is more fun to watch than soccer
Another person at the ESRF which I have rarely seen not smiling is Jos´e
Baruchel. Thank you very much Jos´e for many things: for allowing me to
come to the ESRF as a Master student, for finding some time in your very
busy schedule to discuss the results of our experiments on the ferroelectric
crystals, for accepting to be the president of this jury and especially for the
nice words you had for me during our last meeting in your office and that
I will never forget.
The other part of the joint collaboration between my university in Turin
and the ESRF, which allowed me to come to Grenoble as a Master student,
is due to Prof. Raffaello Garfagnini. Thank you very much for allowing me
to start this adventure in Grenoble, which changed the rest of my life so
deeply.The other Professor at Turin University which I am indebted to is Prof.
Carlo Lamberti. Unfortunately we didn’t succeed in spending a lot of time
together, but every time we met you have been able to, in a balanced way,
compliment me for the results achieved and motivated me for the future
challenges.
I would like to thank Prof. Brian Tanner and Prof. Tilo Baumbach for
accepting the task of reviewing my thesis. Thanks also to Pierre Bastie for to be part of the thesis jury on such short notice.
A special thanks goes to Tamzin Lafford. As I have told you Tamzin, you
have been a kind of Marry Poppins for me. You arrived with many new
ideas which improved considerably the working conditions at the beamline.
Moreover, your dedication in helping me with essentially all my tasks has
been fundamental for the final achievement of my thesis, not to mention
your help in correcting the manuscript. But even more than this, how can I
thank you for the patience which you showed listening to all the rehearsals
of my presentations, the wonderful advice you gave me for my job interviews
and, icing on the cake, your great muffins and delicious cakes you brought
us for our delight? Well, I try with this THANK YOU TAMZIN
Another very important person has been Claudio Ferrero. The amount of
nights we spent together, working on convolution and deconvolution code
has been enormous. But during all this time, you always have managed to
nicely switch between work and pleasant discussions about many different
subjects. Thanks Claudio, even though I will never be able to talk or
understand the dialect from my home town, il piemontese.
This five years spent in Grenoble would not have been the same without
wonderful friends and colleagues, which I will briefly list here: Hedi, Harry,
Rafael, Aymeric, Peter, Michael, David, Sebastien, Xavier, Federico, Gen-
ziana, Pierre-Jean, Valentina, Iulia, Min, Camille, Ali, Eliza,
Grazie ai miei genitori, che con il loro supporto morale ed economico mi
hanno permesso di arrivare fino a qua ed alle mie sorelle, per essere sempre
disponibili ad ascoltarmi ogniqualvolta ho avuto bisogno di qualcuno a cui
parlare.And last, but not least, to my wonderful wife Bibi, to whom this thesis is
dedicated. You have been there for me during the hardest period of my
thesis, the writing-up. Unfortunately, I will not be there for you in the
same hard period, and of that I am deeply sorry; but I hope time will show
us that the decision I took was the good one. To conclude with a happy
thought, I remember that in my Master thesis acknowledgements, I wrote
that I found my diamond in South Africa. Well, I am happy to say that
this diamond will now be with me forever and, with God’s will, it will allow
us to generate even more little diamonds in the futureContents
1 Introduction 1
2 Theoretical basis 5
2.1 Synchrotron radiation . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5
2.1.1 Short historical overview on synchrotron radiation . . . . . . . . 5
2.1.2 Synchrotron radiation properties . . . . . . . . . . . . . . . . . . 8
2.2 X-ray diffraction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12
2.2.1 Kinematical theory of X-ray diffraction . . . . . . . . . . . . . . 12
2.2.2 Dynamical theory of X-ray by a perfect crystal . . . . 13
2.2.2.1 Bragg and Laue cases . . . . . . . . . . . . . . . . . . . 19
2.2.2.2 Asymmetric reflections . . . . . . . . . . . . . . . . . . 22
2.2.2.3 Reflectivity curves in Bragg case . . . . . . . . . . . . . 24
2.3 Coherence . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28
3 Experimental techniques 31
3.1 High Resolution X-ray Diffractometry . . . . . . . . . . . . . . . . . . . 31
3.1.1 Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 31
3.1.2 Determination of apparatus function. . . . . . . . . . . . . . . . . 33
3.1.2.1 Model and fit approach . . . . . . . . . . . . . . . . . . 35
3.1.2.2 Direct deconvolution methods . . . . . . . . . . . . . . 39
3.1.2.3 Comparison of the results obtained. . . . . . . . . . . . 39
3.2 X-ray topography . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 42
3.3 X-ray surface sensitive techniques. . . . . . . . . . . . . . . . . . . . . . 51
3.3.1 X-Ray Reflectivity (XRR) . . . . . . . . . . . . . . . . . . . . . . 52
3.3.2 Grazing Incidence Diffraction (GID) in non-coplanar geometry. . 55
vCONTENTS
4 Characterization of single crystal diamonds 57
4.1 Diamond . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 57
4.1.1 Properties . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 57
4.1.2 Synthesis of diamonds . . . . . . . . . . . . . . . . . . . . . . . . 58
4.2 Characterization of synthetic diamonds. Experimental results. . . . . . . 66
4.2.1 High Resolution X-ray Diffractometry . . . . . . . . . . . . . . . 66
4.2.2 X-ray Topography . . . . . . . . . . . . . . . . . . . . . . . . . . 67
4.2.2.1 White Beam Topography (WBT) . . . . . . . . . . . . 68
4.2.2.2 Double crystal Topography . . . . . . . . . . . . . . . . 71
4.2.2.3 Quantitative analysis of the effective misorientation in
a high quality type IIa diamond . . . . . . . . . . . . . 81
4.2.3 Coherence measurements . . . . . . . . . . . . . . . . . . . . . . 94
4.2.4 Surface sensitive techniques. . . . . . . . . . . . . . . . . . . . . . 100
4.2.4.1 Optical surface profile and AFM results . . . . . . . . . 103
4.2.4.2 Sample preparation . . . . . . . . . . . . . . . . . . . . 105
4.2.5 Grazing Incidence Diffraction . . . . . . . . . . . . . . . . . . . . 106
4.2.6 X-ray Reflectivity . . . . . . . . . . . . . . . . . . . . . . . . . . 108
5 Improvements to polishing of silicon crystals and beryllium windows111
5.1 Improvements and quantification of silicon crystals processing at the
ESRF Crystal Laboratory . . . . . . . . . . . . . . . . . . . . . . . . . . 111
5.1.1 First test - Localization of the main problem. . . . . . . . . . . . 112
5.1.2 Second test - Calibration of the optical polishing. . . . . . . . . . 116
5.1.3 Third test - Optimization of the MCP. . . . . . . . . . . . . . . . 119
5.2 Coherence measurements of the polished samples . . . . . . . . . . . . . 120
5.2.1 Talbot effect measurements . . . . . . . . . . . . . . . . . . . . . 121
5.2.2 Coherence measurements using bi-lens-based interferometer . . . 124
5.3 Improvements on the polishing of beryllium windows . . . . . . . . . . . 128
6 X-ray coherence exploited in imaging of ferroelectric domains 133
6.1 Ferroelectricity . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 133
6.2 Ferroelectric crystals used for non-linear optics applications. . . . . . . . 135
6.3 Visualization of ferroelectric domains using X-ray . . . . . . . . . . . . . 139
6.4 Coherence preserving furnace . . . . . . . . . . . . . . . . . . . . . . . . 140
viCONTENTS
6.5 Visualization of inverted domains in KTA and Rb:KTP crystals. . . . . 144
6.6 Ferroelectric domain behaviour with temperature in Rb:KTP . . . . . . 146
6.7 Conclusions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 152
7 Further diamond related studies 153
7.1 Bending diamonds by femtosecond laser ablation . . . . . . . . . . . . . 153
7.2 X-ray topography of diamond using forbidden reflections: which defects
do we really see? . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 155
7.3 Crystal growth and perfection of large octahedral synthetic diamonds . 157
8 Conclusions 159
References 165
A Apparatus function determination - Direct deconvolution methods III
A.1 Burger - Van Cittert . . . . . . . . . . . . . . . . . . . . . . . . . . . . . III
A.2 Richardson - Lucy . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . VI
viiCONTENTS
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