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Ferroelectric, Pyroelectric and Piezoelectric Effects of Hafnia and Zirconia Based Thin Films

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Ferroelectric, Pyroelectric and Piezoelectric Effects of Hafnia and Zirconia Based Thin Films Ferroelectric, Pyroelectric and Piezoelectric Effects of Hafnia and Zirconia Based Thin Films Von der Fakultät für Elektrotechnik und Informationstechnik der Rheinisch-Westfälischen Technischen Hochschule Aachen zur Erlangung des akademischen Grades eines Doktors der Ingenieurwissenschaften, genehmigte Dissertation vorgelegt von Master of Science Physik Master of Science Elektrotechnik Sergej Starschich aus Duschanbe (Tadschikistan) Berichter: Univ.-Prof. Dr.-Ing R. Waser Apl.-Prof. Dr.-Ing M. Heuken Tag der mündlichen Prüfung: 22.11.2017 Diese Dissertation ist auf den Internetseiten der Hochschulbibliothek online verfügbar. Abstract Ferroelectric materials are of great interest for several applications. On the one hand, the ferroelectric field effect transistor (FeFET) is a promising candidate for future high density, nonvolatile memory devices. On the other hand, in the recent years the energy related applications such as pyroelectric and piezoelectric energy harvesting as well as electrocaloric cooling and electrostatic energy storage attracted wide interest. The conventional ferroelectric materials such as lead zirconatetitanate (PZT) are not completely CMOS compatible and therefore a high-density integration for memory application could not be realized up to date. Furthermore, PZT has environmental issues due to the contained lead. Ferroelectric hafnium oxide, which was first reported in 2011, can overcome the mentioned drawbacks of the conventional ferroelectrics, since it is fully CMOS compatible. The ferroelectric phase is stabilized by doping with various dopants. Furthermore, a mixture of hafnium and zirconium oxide (Hf1-xZrxO2) does also stabilize the ferroelectric phase. In this thesis, hafnia and zirconia based ferroelectrics are deposited by a novel CSD (chemicals solution deposition) process and are characterized in respect to their ferroelectric, piezoelectric and pyroelectric properties. The ferroelectric nature of hafnium oxide is shown for several dopants as well as for Hf1-xZrxO2 with different compositions and for pure ZrO2. Especially in the case of ZrO2 this is very surprising since ZrO2 was studied for many years and for several applications without revealing ferroelectric properties. In contrast to atomic layer deposition (ALD), which is most commonly used for the deposition of hafnia and zirconia based ferroelectric film, the CSD technique is appropriate for deposition of thicker films without a strong reduction of the ferroelectric response. This makes hafnia and zirconia based ferroelectrics suitable for applications, where larger film thicknesses are unavoidable such as piezoelectric and electrocaloric cooling devices. Kurzfassung Ferroelektrische Materialien sind für viele Anwendungsbereiche von großem Interesse. Zum einen ist der ferroelektrische Feldeffekttransistor (FeFET) ein aussichtsreicher Kandidat für zukünftige hochintegrierte nicht flüchtige Speicher. Zum anderen haben energiebezogene Anwendungen wie pyro- und piezoelektrisches Energy Harvesting, elektrokalorisches Kühlen und elektrostatische Energiespeicherung in den letzten Jahren an Bedeutung gewonnen. Die konventionellen Ferroelektrika, wie beispielsweise Blei-Zirkonat-Titanat (PZT), sind nicht CMOS-kompatibel, wodurch eine hohe Integrationsdichte für Speicheranwendungen bis heute nicht erreicht werden konnte. Des Weiteren verursacht PZT Umweltprobleme aufgrund seines Bleigehalts. Mithilfe von ferroelektrischem Hafniumoxid, von dem im Jahre 2011 erstmals berichtet wurde, können die genannten Probleme aufgrund der CMOS-Kompatibilität überwunden werden. Die ferroelektrische Phase kann sowohl durch Dotierung mit verschiedenen Elementen als auch durch eine Zusammensetzung von Hafniumoxid und Zirkoniumoxid (Hf1-xZrxO2) stabilisiert werden. Im Rahmen dieser Arbeit werden auf Hafnium- und Zirconiumoxid basierte Ferroelektrika mittels einer neu entwickelten Routine zur nasschemischen Abscheidung (CSD) hergestellt und hinsichtlich ihrer ferroelektrischen, piezoelektrischen und pyroelektrischen Eigenschaften untersucht. Dabei wird gezeigt, dass sowohl eine Vielzahl von unterschiedlichen Dotierstoffen, als auch für unterschiedliche Zusammensetzungen von Hf1-xZrxO2 sowie für reines ZrO2 die ferroelektrische Phase stabilisiert werden kann. Dies ist besonders überraschend im Fall von ZrO2, welches über Jahre hinweg für unterschiedlichste Anwendungen hin untersucht wurde und dabei keine Anzeichen für Ferroelektrizität gefunden wurden. Im Gegensatz zur Atomlagenabscheidung (ALD), welche am häufigsten zur Deposition von Hafnium- und Zirkonoxid basierten Ferroelektrika genutzt wird, ist die Abscheidung mittels CSD zur Herstellung dicker Schichten geeignet. Dadurch eigenen sich auf Hafnium- und Zirkonoxid basierte Ferroelektrika für Anwendungen, bei denen größere Schichtdicken unumgänglich sind, wie beispielsweise bei piezoelektrischen Sensoren und Aktuatoren sowie beim elektrokalorischen Kühlen. Acknowledgements This thesis was written during my doctoral research at the Institut für Werkstoffe der Elektrotechnik II (IWE 2) at the RWTH Aachen University. First, I would like to thank Prof. Dr. Rainer Waser for the opportunity to work in his research group in the field of novel ferroelectrics. Furthermore, I would like to thank Prof. Dr. Michael Heuken for being the co-examiner of my thesis. I am deeply grateful to Dr. Ulrich Böttger for supervising my work and for countless advices and discussions. I would like to thank my external collaboration partners for the successful cooperation. I appreciated the joint work with the NaMLab group of Dr. Uwe Schröder and Dr. Tony Schenk and the group of Prof. Dr. Alfred Kersch, Robin Materlik and Christopher Künneth from the Munich University of Applied Sciences. I express my gratitude to Dr. Theodor Schneller, and David Griesche for their support especially in the field of solution and sample preparation by use of CSD. Furthermore, I would like to thank Dr. Stephan Menzel for his support as an expert in the field of resistive switching. A big thank you goes to Petra Grewe and Daliborka Erdoglija for spending so much time for the sample preparation and characterization. I would also like to thank Jochen Heiss, Hartmut Pütz and Gisela Wasse for the support in electronics and electron microscopy. For the help and support concerning the images, I am thankful to Thomas Pössinger and Dagmar Leisten. Additionally, I appreciate the administrative support of Martina Heins and Udo Evertz. I also wish to thank my office mates Andreas Burkert, Astrid Marchewka, Inka Nielen, Camilla La Torre, Andreas Kindsmüller and Petra Grewe and all co-workers at the IWE 2 for providing a great working atmosphere. Special thanks go to Sebastian Schmelzer for supervising my Bachelor and Master thesis and for the support during the first month of my thesis. I furthermore acknowledge the helpful support of my student research assistants Bingjie Chen, Jan Lübben, Lucia Lauxmann, Maximilian Geppert, Maximilian Kühn, Nan Zhang, Parisa Jaberi, You-Ron Lin and Charlotte Böttger. Contents 1 Introduction 1 2 Fundamentals 3 2.1 Crystal Structure ................................................................................ 3 2.2 Ferroelectricity ................................................................................... 4 2.3 Pyroelectricity .................................................................................... 6 2.4 Piezoelectricity ................................................................................... 7 2.5 Resistive Switching ............................................................................ 8 2.6 Ferroelectric Field Effect Transistor .................................................. 9 2.7 Physical Basics of Sputtering ........................................................... 11 2.8 Experimental Methods ..................................................................... 12 3 Sample Preparation 23 3.1 Electrodes and Oxide Sputtering ...................................................... 23 3.2 Chemical Solution Deposition ......................................................... 25 4 Ferroelectric and Piezoelectric Properties of HZO and ZrO₂ 39 4.1 Composition dependence ................................................................. 41 4.2 Ferroelectric ZrO₂ ............................................................................ 46 4.3 Doped ZrO2 ...................................................................................... 51 5 Ferroelectric Properties of Doped HfO₂ 59 5.1 Sputtered yttrium doped HfO₂ .......................................................... 60 5.2 CSD prepared yttrium doped HfO2 .................................................. 64 5.3 Further Dopants ................................................................................ 68 6 Wake-up and Degradation 81 6.1 Wake-up ........................................................................................... 81 6.2 Degradation and fatigue ................................................................... 96 7 Pyroelectric Properties 101 7.1 Yttrium Doped Hafnium Oxide ..................................................... 102 7.2 Pure Zirconium Oxide .................................................................... 104 7.3 Figures of merit .............................................................................. 107 8 Conclusions 109 8.1 Summary ........................................................................................ 109 8.2 Outlook ..........................................................................................
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