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III-V Semiconductor Structures for Biosensor and Molecular Electronics Applications

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III-V Semiconductor Structures for Biosensor and Molecular Electronics Applications Lehrstuhl für experimentelle Halbleiterphysik I Walter Schottky Institut Technische Universität München III-V Semiconductor Structures for Biosensor and Molecular Electronics Applications Sebastian M. Luber Vollständiger Abdruck der von der Fakultät für Physik der Technischen Universität München zur Erlangung des akademischen Grades eines Doktors der Naturwissenschaften genehmigten Dissertation. Vorsitzender: Univ.-Prof. Dr. Roland Netz Prüfer der Dissertation 1. Univ.-Prof. Dr. Gerhard Abstreiter 2. Univ.-Prof. Paolo Lugli, Ph. D. Die Dissertation wurde am 13.07.2006 bei der Technischen Universität München eingereicht und durch die Fakultät für Physik am 18.10.2006 angenommen. 1. Auflage Januar 2007 Copyright 2007 by Verein zur Förderung des Walter Schottky Instituts der Technischen Universität München e.V., Am Coulombwall, 85748 Garching. Alle Rechte vorbehalten. Dieses Werk ist urheberrechtlich geschützt. Die Vervielfältigung des Buches oder von Teilen daraus ist nur in den Grenzen der geltenden gesetzlichen Bestimmungen zulässig und grundsätzlich vergütungspflichtig. Titelbild: The left panel of the cover picture demonstrates the operational principle of a gallium arsenide based biosensor. The analyte binds to a receptor molecule which is embedded in a biphenyl functional layer on the sensor surface. This binding event is detected by a shallow two dimensional electron gas which is sensitive to surface potential changes. The right panel illustrates a similar semiconductor structure which was used for molecular electronics experiments. Organic pi-conjugated molecules are attached to nanometer spaced electrodes which have been previously deposited on a cleaved heterostructure. Thereby, the current carrying properties of the molecules can be evaluated. Druck: Printy Digitaldruck, München (http://www.printy.de) ISBN: 978-3-932749-83-4 Für Nicola und Maja Zusammenfassung Die vorliegende Arbeit beschäftigt sich mit der Verwendung von elektronischen, auf III-V Halbleitern basierenden Bauelementen für die Biosensorik und die molekulare Elektronik. Da- zu wird im ersten Teil ein Sensor, der aus einem oberflächennahen, zweidimensionalen Elek- tronengas in einer Aluminiumgalliumarsenid-Galliumarsenid (AlGaAs-GaAs) Heterostruktur besteht, für eine Anwendung in biologischer Umgebung untersucht. Zur Stabilisierung in dabei vorkommenden wässrigen Lösungen wird der Sensor mit einer geordneten organischen Schicht aus substituierten Mercaptobiphenyl-Molekülen passiviert. Der Einfluss dieser Moleküle auf die elektronische Struktur der GaAs-Oberfläche wird daraufhin anhand von Kelvin-Probe Messun- gen in Luft diskutiert. Dabei wird eine Abhängigkeit der Elektronenaffinität vom intrinsischen molekularen Dipolmoment der Mercaptobiphenyle festgestellt. Des Weiteren werden zeitauf- gelöste Messungen präsentiert, die einen Einfluss der Mercaptobiphenyl-Beschichtung auf die Ladungsträgerrekombination zeigen. Bei einer Charakterisierung in physiologischen Pufferlö- sungen zeigt sich dann anhand von Leitfähigkeitsmessungen eine Abhängigkeit des Sensor- Oberflächenpotenzials von pH-Wert und Salzgehalt der Elektrolytlösung. Durch Simulations- rechnungen unter Verwendung der Poisson-Boltzmann Theorie ergeben sich als mögliche Ursa- chen sowohl eine Bindung von OH- Ionen an die Oberfläche, als auch die Dissoziation von OH Gruppen in Oberflächenoxiden. Ein Vergleich zwischen Simulationsparametern und physika- lischer Beschaffenheit des Sensors deutet dabei auf die OH- Absorption als wahrscheinlichere Ursache hin. Im zweiten Teil der Arbeit wird die Eignung von MBE gewachsenen III-V Halbleiterstruk- turen für die molekulare Elektronik untersucht. Dabei wird eine Methode für die Herstellung metallischer Elektroden im Abstand von wenigen Nanometern auf einer GaAs-AlGaAs Träger- struktur präsentiert und erfolgreich produzierte Strukturen topographisch und elektrisch unter- sucht. Die erfolgreiche Funktion des Bauelements wird dabei durch das Einfangen einzelner Gold-Nanopartikel demonstriert. Eine erste Anwendung für die molekulare Elektronik wird durch die elektrische Charakterisierung von molekularen Schichten aus Oligophenylenvinylen- Derivaten aufgezeigt. Simulationen an vereinfachten Molekülen mittels erweiterter Hückel Theo- rie und der Methode der Greens-Funktionen zeigen eine gute qualitative Übereinstimmung zwi- schen Theorie und Experiment. Außerdem werden viel versprechende Erweiterungen der Her- stellungsmethode präsentiert. Diese umfassen die Fabrikation von T-strukturierten Elektroden zur Untersuchung einzelner Moleküle, und den Übergang zu reinen Halbleiterelektroden beste- hend aus Indiumarsenid Schichten. I Abstract The present work reports on the employment of III-V semiconductor structures to biosensor and molecular electronics applications. In the first part a sensor based on a surface-near two di- mensional electron gas for a use in biological environment is studied. Such a two dimensional electron gas inherently forms in a molecular beam epitaxy (MBE) grown, doped aluminum gallium arsenide - gallium arsenide (AlGaAs-GaAs) heterostructure. Due to the intrinsic insta- bility of GaAs in aqueous solutions the device is passivated by deposition of a monolayer of 4’-substituted mercaptobiphenyl molecules. The influence of these molecules which bind to the GaAs via a sulfur group is investigated by Kelvin probe measurements in air. They reveal a dependence of GaAs electron affinity on the intrinsic molecular dipole moment of the mercap- tobiphenyls. Furthermore, transient surface photovoltage measurements are presented which demonstrate an additional influence of mercaptobiphenyl chemisorption on surface carrier re- combination rates. As a next step, the influence of pH-value and salt concentration upon the sensor device is discussed based on the results obtained from sensor conductance measurements in physiological solutions. A dependence of the device surface potential on both parameters due to surface charging is deduced. Model calculations applying Poisson-Boltzmann theory reveal as possible surface charging mechanisms either the adsorption of OH- ions on the surface, or the dissociation of OH groups in surface oxides. A comparison between simulation settings and physical device properties indicate the OH- adsorption as the most probable mechanism. In the second part of the present study the suitability of MBE grown III-V semiconduc- tor structures for molecular electronics applications is examined. In doing so, a method to fabricate nanometer separated, coplanar, metallic electrodes based on the cleavage of a support- ing AlGaAs-GaAs heterostructure is presented. This is followed by a thorough topographical and electrical characterization of fabricated devices which includes the electrostatic trapping of single gold nanoclusters between the electrodes. A first application to molecular electron- ics is presented by conductance measurements on a molecular layer of oligophenylenvinylene derivatives. Simulations on model molecules applying extended Hückel theory and the non- equilibrium Greens function formalism reveal a good qualitative agreement between theory and experiment. Furthermore, promising extensions to the present fabrication method are discussed. These include the processing and characterization of broken T-shaped electrodes suitable for measurements on single molecules, and the transition to pure semiconductor electrodes based on indium arsenide. II Table of Contents Motivation and Outline 1 I Gallium Arsenide Based Devices for Biosensing Applications 5 1 Introduction 7 1.1 The Sensor Element - A Two Dimensional Electron Gas ............ 9 1.2 Sensor Passivation and Functionalization ..................... 10 2 Fundamentals of Semiconductors in Electrolytes 13 2.1 Semiconductor Surface Electronic Structure ................... 13 2.1.1 The GaAs Surface ............................ 15 2.1.2 Influence of Chemisorbed Molecules .................. 15 2.2 Buffered Electrolyte Solutions .......................... 17 2.2.1 Buffer Action ............................... 18 2.2.2 Effect of Temperature and Ionic Strength ................ 19 2.2.3 Phosphate Buffers ............................ 19 2.3 Semiconductor-Electrolyte Interface ....................... 19 2.3.1 Poisson-Boltzmann Theory ........................ 21 2.3.2 Site-Dissociation Theory ......................... 25 2.3.3 Alternative Adsorption Models ...................... 28 2.3.4 Capacitance and Mott-Schottky Analysis ................ 29 2.4 Numerical Calculations .............................. 31 2.4.1 Simulation of the Semiconductor Electrolyte Interface ......... 31 2.4.2 Simulation of Molecular Properties ................... 35 III IV Contents 3 Experimental Techniques and Measurement Setup 39 3.1 Sample Design and Fabrication .......................... 39 3.1.1 Molecular Beam Epitaxy Growth .................... 40 3.1.2 Device Layout and Patterning ...................... 40 3.1.3 Deposition of Mercaptobiphenyl Monolayers .............. 41 3.2 Experimental Setup and Measurement Details .................. 42 3.2.1 Kelvin Probe Measurements ....................... 42 3.2.2 Electrochemical Setup and Fluid Handling ............... 45 3.2.3 Transport Measurements ......................... 46 3.2.4 Impedance Measurements ........................ 48 4 Surface Electronic Structure Changes of GaAs by Molecular Adsorption 51 4.1 Influence of Mercaptobiphenyl Deposition on Work Function and Band Bending 51 4.2 Electron Affinity Changes Upon Mercaptobiphenyl Adsorption ......... 53 4.3 Surface
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