Synthesis and characterization of carbon nanotube-reinforced copper thin films [Elektronische Ressource] / vorgelegt von Cornelia Otto

Synthesis and characterization of carbon nanotube-reinforced copper thin films [Elektronische Ressource] / vorgelegt von Cornelia Otto

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Max-Planck-Institut für Metallforschung Stuttgart Synthesis and Characterization of Carbon Nanotube-Reinforced Copper Thin Films Cornelia Otto Dissertation an der Universität Stuttgart Bericht Nr. 194 November 2006 Synthesis and CharacterizationofCarbon Nanotube-Reinforced Copper Thin FilmsVon der Fakultät Chemie der Universität Stuttgartzur Erlangung der Würde eines Doktors derNaturwissenschaften (Dr. rer. nat.) genehmigte Abhandlungvorgelegt vonCornelia Ottoaus MühlackerHauptberichter: Prof. Dr. E. ArztMitberichter: Prof. Dr. M. RühleTag der mündlichen Prüfung: 16. November 2006Max-Planck-Institut für Metallforschung, Stuttgart2007Für StephanThe cover picture shows carbon nanotubes which had been modi-fied chemically before being used in an electrolysis experiment. Inthe course of this experiment, carbon from the graphite anode de-posited at the modified sites. Scientifically, this experiment turnedout to be a dead end, but the samples provided beautiful images,and the image shown here won the 2006 Nano&Arts competition.7AcknowledgementsA dissertation is too heavy a load for one person alone. Many people have helpedme in the course of the past three years and I am much indebted to all of them.First of all, I want to thank Prof. Eduard Arzt as my advisor and Prof.

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Max-Planck-Institut für Metallforschung
Stuttgart

Synthesis and Characterization of Carbon Nanotube-
Reinforced Copper Thin Films

Cornelia Otto
Dissertation
an der
Universität Stuttgart

Bericht Nr. 194
November 2006 Synthesis and Characterization
of
Carbon Nanotube-Reinforced Copper Thin Films
Von der Fakultät Chemie der Universität Stuttgart
zur Erlangung der Würde eines Doktors der
Naturwissenschaften (Dr. rer. nat.) genehmigte Abhandlung
vorgelegt von
Cornelia Otto
aus Mühlacker
Hauptberichter: Prof. Dr. E. Arzt
Mitberichter: Prof. Dr. M. Rühle
Tag der mündlichen Prüfung: 16. November 2006
Max-Planck-Institut für Metallforschung, Stuttgart
2007Für Stephan
The cover picture shows carbon nanotubes which had been modi-
fied chemically before being used in an electrolysis experiment. In
the course of this experiment, carbon from the graphite anode de-
posited at the modified sites. Scientifically, this experiment turned
out to be a dead end, but the samples provided beautiful images,
and the image shown here won the 2006 Nano&Arts competition.7
Acknowledgements
A dissertation is too heavy a load for one person alone. Many people have helped
me in the course of the past three years and I am much indebted to all of them.
First of all, I want to thank Prof. Eduard Arzt as my advisor and Prof. Manfred
RühleasthechairmanoftheGraduiertenkollegwhichprovidedmyfinancialsupport.
Without them, this dissertation would not have been possible.
Over the course of my dissertation, four scientists have advised me in all arising
problems and provided encouragement and fruitful discussion. I am deeply grateful
for all their help. In chronological order, these four were Dr. Nicole Grobert, Dr.
John Balk, Dr. Gerhard Dehm and finally Dr. Julie Nucci, who took the longest
turn.
The thin films group of the department Arzt was always a good platform for
discussing new results. Thank you for listening so patiently to all my nanotubes
problems even if they didn’t concern your own work.
Dr. Andrei Matveev and his knowledge on electrodeposition were of immeasur-
able help for the studies on the eletcrolytically produced samples. Thank you very
much.
Dr. Steffen Orso, Dr. Gunther Richter, Ulrike Eigenthaler and Birgit Heiland
helped me immensely in making some last-minute samples. With all my heart I
appreciate the effort they have made, finding time for my samples at short notice
and running late hours. In addition, I want to thank all the technicians who have
helped me with their expertise and experience and also Mrs. Hess for all her help
in administrative matters.8
I want to thank Linda, who has shared my problems and successes since our first
day at the university, my office mates Tobi, Petra and Chris, the Max-Planck role
playing group and all my colleagues at the department for their friendship and for
all the good times we had together.
Finally, I want to thank my parents, my brother and my godfather for their
support during the three years of the dissertation and all the time before. But my
deepest love and gratefulness goes to my husband Stephan, who has supported me
and endured me when the stress got to me. This work is dedicated to him.9
Contents
Contents 9
List of symbols and abbreviations 13
Deutsche Zusammenfassung 15
Abstract 27
1 Introduction 29
2 Literature Review 31
2.1 Carbon nanotubes . . . . . . . . . . . . . . . . . . . . . . . . . . . . 31
2.1.1 Structure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 31
2.1.2 Production methods . . . . . . . . . . . . . . . . . . . . . . . 34
2.1.3 Mechanical properties . . . . . . . . . . . . . . . . . . . . . . 37
2.1.4 Wetting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 42
2.1.5 Nitrogen doping . . . . . . . . . . . . . . . . . . . . . . . . . . 43
2.2 Composites . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 46
2.2.1 Composite theory . . . . . . . . . . . . . . . . . . . . . . . . . 46
2.2.2 Composites with CNTs . . . . . . . . . . . . . . . . . . . . . . 50
2.2.3 Metal matrix composites with CNTs . . . . . . . . . . . . . . 51
2.3 Motivation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 56
3 Carbon nanotubes in sputtered copper films 59
3.1 Motivation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 59
3.2 Experimental Procedure . . . . . . . . . . . . . . . . . . . . . . . . . 60
3.2.1 Synthesis of CNTs . . . . . . . . . . . . . . . . . . . . . . . . 60
3.2.2 Parameters for the deposition of the copper layers . . . . . . . 62
3.2.3 Deposition of nanotubes . . . . . . . . . . . . . . . . . . . . . 6310 CONTENTS
3.2.4 Dispersing nanotubes . . . . . . . . . . . . . . . . . . . . . . . 63
3.2.5 Deposition Methods . . . . . . . . . . . . . . . . . . . . . . . 64
3.3 Results . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 66
3.3.1 Quality of nanotube dispersion . . . . . . . . . . . . . . . . . 67
3.3.2 Conformity . . . . . . . . . . . . . . . . . . . . . . . . . . . . 67
3.4 Discussion and Outlook. . . . . . . . . . . . . . . . . . . . . . . . . . 71
4 Cu/CN microcolumns: compression testing and TEM analysis 75x
4.1 Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 75
4.2 Experimental procedure . . . . . . . . . . . . . . . . . . . . . . . . . 78
4.2.1 Preparation of micron-sized columns . . . . . . . . . . . . . . 78
4.2.2 In situ compression testing . . . . . . . . . . . . . . . . . . . . 79
4.2.3 Ex situ testing . . . . . . . . . . . . . . . . . . . 80
4.2.4 Preparation of TEM specimens and TEM analysis . . . . . . . 81
4.3 Results and discussion . . . . . . . . . . . . . . . . . . . . . . . . . . 82
4.3.1 Stress-strain measurements . . . . . . . . . . . . . . . . . . . . 84
4.3.2 Matrix deformation mechanisms . . . . . . . . . . . . . . . . . 88
4.3.3 Matrix-nanotube interactions . . . . . . . . . . . . . . . . . . 94
4.4 Summary and outlook . . . . . . . . . . . . . . . . . . . . . . . . . . 100
5 Preferential deposition of copper on CNTs 105
5.1 Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 105
5.2 Experimental procedure . . . . . . . . . . . . . . . . . . . . . . . . . 106
5.2.1 Isolated CN on copper . . . . . . . . . . . . . . . . . . . . . 106x
5.2.2 Aligned CNT-carpets on non-conductive substrate . . . . . . . 107
5.2.3 Tangledets on conductive substrate . . . . . . . . . 108
5.3 Results . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 108
5.3.1 Isolated CN on copper . . . . . . . . . . . . . . . . . . . . . 108x
5.3.2 Aligned CNT-carpets on non-conductive substrate . . . . . . 109
5.3.3 Tangledets on conductive substrate . . . . . . . . . 112
5.4 Discussion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 115
5.4.1 Samples with isolated CN . . . . . . . . . . . . . . . . . . . . 115x
5.4.2 Samples with CNT-carpets . . . . . . . . . . . . . . . . . . . . 115
5.5 Summary and outlook . . . . . . . . . . . . . . . . . . . . . . . . . . 117