From molecular building blocks to condensed carbon nitride networks [Elektronische Ressource] : structure and reactivity / Bettina Valeska Lotsch

Bettina Valeska Lotsch

Informations

• Publié par: ludwig-maximilians-universitat_munchen
• Publié le: 01 janvier 2006
• Nombre de lectures: 45
• Langue: English
• Poids de l'ouvrage: 12 Mo

Extrait

Dissertation zur Erlangung des Doktorgrades
der Fakult¨ at fur¨ Chemie und Pharmazie
der Ludwig-Maximilians-Universit¨ at Munc¨ hen
From Molecular Building Blocks to
Condensed Carbon Nitride Networks:
Structure and Reactivity
Bettina Valeska Lotsch
aus
Frankenthal /Pfalz
2006Erkl¨arung
Diese Dissertation wurde im Sinne von § 13 Abs. 3 bzw. 4 der Promotionsordnung vom 29.
Januar 1998 von Herrn Prof. Dr. Wolfgang Schnick betreut.
Ehrenwortlic¨ he Versicherung
Diese Dissertation wurde selbstst¨ andig, ohne unerlaubte Hilfe erarbeitet.
M¨ unchen, den 20. 11. 2006
Bettina Valeska Lotsch
Dissertation eingereicht am 20.11. 2006
1. Gutachter: Prof. Dr. Wolfgang Schnick
2. Gutachter: Prof. Dr. Jurgen¨ Senker
M¨ undliche Prufung¨ am 19.12. 2006To my parents
and sisterAcknowledgements
First of all, I would like to express my gratitude to Prof. W. Schnick for giving me the op-
portunity to work in his group, for the freedom of research paired with continuous advertence
and support, and for his stimulating enthusiasm. Without his professional guidance and en-
couragement, this thesis would not have become what it is.
I am indebted to Prof. J. Senker for introducing me into the “brave new world” of solid-state
NMR, for his encouragement to never stop digging deeper, for his conviction that the time
issue comes only second, and for his seemingly never ending repertoir of questions, answers,
ideas and patience, as well as for being co-referee of this thesis.
I am thankful to Prof. T. Bein, Prof. D. Johrendt, Prof. K. Karaghiosoff and Prof. T. M.
Klap¨ otke for their being available as examiners in my viva-voce.
Special thanks go to Dr. Markus Doblinger,¨ as well as Lena Seyfarth and Jan Sehnert for a
fruitful collaboration and stimulating insights into electron diffraction, solid-state NMR, and
the world of theory, respectively.
For carrying out innumerous measurements, as well as for the “postprocessing” involved, I
would like to thank Sandra Albert, Dr. Sascha Correll, Dr. Markus Doblinger,¨ Dagmar Ewald,
Dr. Gerd Fischer, Helmut Hartl, Dr. Alexandra Lieb, Prof. Dr. Konstantin Karaghiosoff,
Juliane Kechele, Thomas Miller, Christian Minke, Peter Mayer, Dr. Peter Mayer, Dr. Oliver
Oeckler, Andreas Sattler and Wolfgang Wunsc¨ hheim.
In detail, I would like to thank
• Dr. Oliver Oeckler for his invaluable advice (both in real and in reciprocal space) and
for his particular “challenging” view on things in general,
• Dr. Jorn¨ Schmedt auf der Gunne¨ and Christian Minke for their assistance and co-
operation in all NMR-related matters,
• Dr. Barbara Jurgens¨ for opening up the intriguing playground of C/N chemistry and
shifting the focus to the most interesting problems,
• Andreas Sattler and Theresa Soltner for their assistance, invaluable discussions and
exchange of views on C/N matters and beyond,• my bachelor and research students Lucia Romana Lorenz and Daniel Benker for their
participation and support,
• Carolin Buhtz for her creative contributions to the electron diffraction investigations
and her imperturbable capability to listen and de-dramatize things,
• Dr. Alexandra Lieb for keeping company in our “night-lab”, for her unfailing nutritional
backup, and for her inspiringly different world outlook – I learned a lot...
• Dr. Ulrich Baisch and Dr. Sascha Correll for their outstanding helpfulness and guidance,
• Dr. Alexandra Lieb, Juliane Kechele, Robert Kraut, Dr. Abanti Nag, Rebecca R¨ omer
and Wolfgang Wunsc¨ hheim for their collegiality and for creating a pleasant working-
and “biosphere” in laboratory D 2.107,
• Wolfgang Wunsc¨ hheim for technical support whenever hardware or software of all kinds
quit the service,
• Richard Betz, Sebastian Braun, Dr. Markus Doblinger,¨ Michael Gob¨ el and Dr. Oliver
Oeckler for proof-reading this thesis and for racking their brains for me ...
For providing a particularly convenient working atmosphere throughout the last years and for
all sorts of technical, scientific and “personal” support, I woud like to thank my – present and
past – colleagues Dr. Ulrich Baisch, Constantin Beyer, Sabine Beyer, Daniel Bichler, Cordula
Braun, Sascha Correll, Holger Emme, Cora Hecht, Elsbeth Hermanns, Gunther Heymann, Dr.
Henning H¨ oppe, PD Dr. Hubert Huppertz, Stefanie Jakob, Petra Jakubcova, Friedrich Ka-
rau, Juliane Kechele, Johanna Knyrim, Robert Kraut, Dr. Alexandra Lieb, Catrin L¨ ohnert,
Thomas Miller, Christian Minke, Helen Muller,¨ Dr. Abanti Nag, Dr. Oliver Oeckler, Sandro
Pagano, Dr. Regina Pocha, Florian Pucher, Stefan Rannabauer, Christoph R¨ ohlich, Rebecca
R¨ omer, Andreas Sattler, Dr. Jorn¨ Schmedt auf der Gunne,¨ Christian Schmolke, Stefan Sedl-
maier, Jan Sehnert, Lena Seyfarth, Theresa Soltner, Florian Stadler, Dr. Johannes Weber,
Wolfgang Wunsc¨ hheim and Martin Zeuner.Above all, I am indebted to my parents, my sister and Sebastian, who continuously encouraged
and supported me with maximum forbearance and patience. For all what they have done and
sacrificed, suffice it to say:
Gratitude is one of the least articulate of the emotions, especially when it is deep.
Felix FrankfurterBe not afraid of growing slowly, be afraid only of standing still.
Chinese ProverbContents
1 Introduction 15
2 Experimental Methods 22
2.1 PreparativeMethods................................. 22
2.1.1 VacuumandInertGasLine......................... 22
2.1.2 Furnaces.................................... 22
2.1.3 GloveBox................................... 23
2.1.4 OperatingTechniques............................ 23
2.2 AnalyticalMethods.................................. 24
2.2.1 DiffractionTechniques 24
2.2.2 SpectroscopicMethods 30
2.2.3 ElementalAnalysis.............................. 36
2.2.4 MasSpectrometry 37
2.2.5 ThermalAnalysis............................... 37
3 Theoretical Basis and Models 38
3.1 DynamicalProceses................................. 38
3.2 NeutronScatering.................................. 41
3.2.1 BasicPrinciples 41
3.2.2 Diffraction 43
3.2.3 QuasielasticNeutronScatering(QENS).................. 44
3.2.4 MotionalModels............................... 46
3.2.5 EISF...................................... 47
3.3 MagneticResonance................................. 48
3.3.1 BasicPrinciples 48
3.3.2 InteractionHamiltoniansandOperatorFormalism............ 50
3.3.3 High-ResolutionNMR:GeneralAspectsandTechniques......... 63
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