Thèse présentée pour obtenir le grade de Docteur de lUniversité Louis Pasteur
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Thèse présentée pour obtenir le grade de Docteur de lUniversité Louis Pasteur

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Niveau: Supérieur, Doctorat, Bac+8
Thèse présentée pour obtenir le grade de Docteur de lUniversité Louis Pasteur Strasbourg I Discipline: Chimie Physique par Marianne Gaborieau Solid-state NMR investigation of spatial and dynamic heterogeneity in acrylic pressure sensitive adhesives (PSAs) compared to model poly(n-alkyl acrylates) and poly(n-alkyl methacrylates) Soutenue publiquement le 10 mars 2005 Membres du Jury : Directeur de Thèse: M. Bernard Meurer, Chargé de Recherche, Strasbourg Rapporteur Interne : M. Gilbert Weill, Professeur Emérite, Université Strasbourg I Rapporteur Externe : Mme Bernadette Charleux, Professeur, Université Paris VI Rapporteur Externe : M. Piotr Tekely, Directeur de Recherche, Nancy Examinateur : M. Hans Wolfgang Spiess, Professeur, Université de Mayence, Allemagne Examinateur : M. René-Paul Eustache, Ingénieur de Recherche, Arkema

  • many nice evenings

  • grade de docteur de luniversité

  • polymer physics

  • state nmr

  • nancy examinateur

  • dsc measurements

  • nmr problems

  • directeur de la recherche


Sujets

Informations

Publié par
Publié le 01 mars 2005
Nombre de lectures 64
Langue English
Poids de l'ouvrage 7 Mo

Extrait


Thèse présentée pour obtenir le grade de
Docteur de l´Université Louis Pasteur
Strasbourg I

Discipline: Chimie Physique
par Marianne Gaborieau






Solid-state NMR investigation
of spatial and dynamic heterogeneity
in acrylic pressure sensitive adhesives (PSAs)
compared to model poly(n-alkyl acrylates)
and poly(n-alkyl methacrylates)









Soutenue publiquement le 10 mars 2005


Membres du Jury :

Directeur de Thèse: M. Bernard Meurer, Chargé de Recherche, Strasbourg
Rapporteur Interne : M. Gilbert Weill, Professeur Emérite, Université Strasbourg I
Rapporteur Externe : Mme Bernadette Charleux, Professeur, Université Paris VI e : M. Piotr Tekely, Directeur de Recherche, Nancy
Examinateur : M. Hans Wolfgang Spiess, Professeur, Université de Mayence, Allemagne
Examinateur : M. René-Paul Eustache, Ingénieur de Recherche, Arkema





Voici le terme d’un long périple
dans l’espace et dans le temps.

This is the end of a long travel through Space and Time.
Marc Gaborieau, Le Népal, une introduction à la connaissance du monde népalais,
Kailash éditions, Paris, 1995, p. 291






La verdadera ciencia enseña, sobre todo,
a dudar y a ser ignorante.

True science teaches, above all, to doubt and to be ignorant.
Miguel de Unamuno, Tragic sense of life, 1913










†à Marc et Catherine , Thomas, Julie et Capucine
à Patrice ...

i
ii Acknowledgements

Thanks are due to Bernard Meurer for accepting the official supervision of this work .
I would like to gratefully acknowledge Hans W. Spiess for allowing me to conduct my PhD work in his
research group at the Max Planck Institute for Polymer Research (Mainz, Germany). This was a fruitful
experience on a scientific as well as on a human point of view. I benefited from his never failing and
motivating support.
I would like to thank Manfred Wilhelm for his supervision at the beginning of this work, for his readiness
to answer my questions on various topics: science, Riesling, Pfalz...
Special thanks to Robert Graf for the never failing assistance concerning all practical spectrometer and
NMR problems, for enlightening discussions about polymer physics, for careful reading of the manuscript
and help for final corrections, as well as for many nice evenings around a good meal with Katharina ...
I am indebted to Atofina for financial support and for providing the investigated pressure sensitive
adhesive samples, to François Beaume for interesting discussions, to René-Paul Eustache, Stéphane
Lepizzéra, Françoise Cochet and Olivier Colombani for the interest they take in my project.

I am grateful to Bernadette Charleux, Gilbert Weill, and Piotr Tekely for accepting to read this manuscript
and report on this work.
Thanks are due to Nawel Khelfallah and Gilbert Weill for helping me organizing the defense.

I am very grateful to Mario Beiner from the University of Halle Wittenberg (Germany) for his invitation
and nice welcome in Halle, for numerous and fruitful disciussions. My chemist point of view of the
nanophase separation was enlightened by his physicist experience.

I would like to thank Prof. Pakula for a friendly and fruitful cooperation on local dynamics in
polyacrylates, and Stefan Kahle for numerous dielectric relaxation measurements, analysis and
explanations.


In a random order, I would like to express many thanks to the Spiess group and the MPI-P, in particular:

Uta Pawelzik for her kind help during the poly(n-alkyl acrylates) synthesis and an introduction to various
characterization techniques
Verona Maus for many urgent DSC measurements and friendly discussions
The "Chemielabor" team for the nice working atmosphere : Uli Jonas, the Neidhöfers, Kiki, Arancha, Diane,
Diana, Michelle, Silvia, Petra, Charles-André, etc.

iiiMichael Neidhöfer, Axel Kretschmer, Robert Graf and Ingrid Fischbach for their patient explanations of
the way of operating a spectrometer, and how to properly record NMR data
Katja Klimke and Matt Parkinson for the precious advices and experimental tricks concerning the
branching quantification
Manfred Hehn, Hans Peter Reich for the efficient technical assistance with spectrometers, for always
finding solutions to the problems arising from annoying samples, mechanics or electronics
Frank Keller for computer assistance on a French-speaking laptop with French keyboard

The unforgettable 3M team of the Massenzimmer: Mark McCormick, Matt Parkinson, Michael Pollard,
for my big progress in English language, journeys in time, Jazz-and-beer evenings, discussions about NMR
(what about that Mainz 05?) and more, and making me feel at home ... I thank them also, as well as Attila
Domján, Sheng-Shu Hou, Christian Krüger, Diana Boos, Timm Doetsch for the nice working atmosphere in
room of Massen and Zimmer
Ingrid Fischbach, Katja Klimke, Michael Neidhöfer, for a friendly time together by Bürochef and Alumni

Barbara Doerner-Stute, the good soul of the Spiess group, for her kindness, her patience, her continuous
help concerning administrative and morale things.
Corinna Kautz for successfully continuing this difficult task.

Michael Wind for providing the poly(n-alkyl methacrylates) samples together with the characterization of
the dynamic heterogeneity, and tricks for low temperature measurements.

The Spiess group and the MPI-P in general for the multicultural experience: among others Gillian from
Canada, Erli from Indonesia, Alexandra from Italy, Eva from Spain, Han-Bong from Korea/Saarland,
Grazyna from Poland, Julia form Russia/America/Israel, Shi Feng from China, Sanjay from
India/Netherlands, Yao from China, Doene, Fatma, Mehmet and Bahar from Turkey, Juana and Carlos
from Mexico, Rafa from Catalonia, Laurent and Baptiste from France, Britt from the USA, Karen and
Michael from Germany...

Frau Nanz for many urgent printing / cuting / binding


I am grateful to my parents and brother and sisters for encouraging higher studies in a field foreign to them
(“and at the end you will tell us why the adhesives stick ?”), my grandmother for many phone calls.
A very special thank goes to Patrice for his continuous and attentive help, from countless 6h train trips to
careful reading of solid-state NMR or dynamics study, and so much more ...

I would like to apologize to all the ones I did not have enough space or memory to namely thank...
iv Table of contents


Résumé de la thèse...............................................................................................ix
I. Introduction .......................................................................................................ix
A. Contexte.................................................................................................................ix
B. Présentation des échantillons ...................................................................................x
C. Démarche...............................................................................................................xi
II. Etude du branchement......................................................................................xi
A. Etat de l’art.............................................................................................................xi
13B. Quantification du branchement par RMN C ....................................................... xi
C. Détection des branches longues par SEC multi-détection .................................... xii
III. Filtre dipolaire et dynamique locale dans des polymères fondus ...............xiii
A. Présentation des échantillons étudiés................................................................... xiii
1B. Technique de diffusion de spin H nucléaire avec filtre dipolaire....................... xiv
C. Contraste dynamique dans les PnAAs et PnAMAs fondus ...................................xv
D. Sélection réelle et mécanisme de diffusion de l’aimantation.................................xv
E. Quantification de la dynamique locale................................................................. xvi
F. Interprétation des résultats .................................................................................. xvii
G. Comparaison de tous les échantillons ................................................................ xviii
IV. Conclusion générale et perspectives ............................................................xviii
V. Plan du manuscrit de thèse.............................................................................xix
Part 0: General introduction................................................................................ 1
Part 1: Literature survey and motivation 5
7-10I. Pressure sensitive adhesive materia

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