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Wide Band Gap Materials and Devices for Nox, H2 and O2 Gas Sensing Applications

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Wide Band Gap Materials and Devices for Nox, H2 and O2 Gas Sensing Applications Wide band gap materials and devices for NOx, H2 and O2 gas sensing applications Dissertation zur Erlangung des akademischen Grades Doktor-Ingenieur (Dr.-Ing.) vorgelegt der Fakultät Elektrotechnik und Informationstechnik der Technischen Universität Ilmenau von Dipl.-Ing Majdeddin Ali geboren am 08.09.1976 in Homs, Syrien 1. Gutachter: Univ.-Prof. Dr. rer. nat. habil. Oliver Ambacher, Fraunhofer-Institut für Angewandte Festkörperphysik, Freiburg 2. Gutachter: PD Dr.-Ing. habil. Frank Schwierz, TU Ilmenau 3. Gutachter: Dr. Martin Eickhoff, Walter Schottky Institut, TU München Tag der Einreichung: 28.06.2007 Tag der wissenschaftlichen Aussprache: 22.01.2008 urn:nbn:de:gbv:ilm1-2007000323 Abstract III Abstract In this thesis, field effect gas sensors (Schottky diodes, MOS capacitors, and MOSFET transistors) based on wide band gap semiconductors like silicon carbide (SiC) and gallium nitride (GaN), as well as resistive gas sensors based on indium oxide (In2O3), have been developed for the detection of reducing gases (H2, D2) and oxidising gases (NOx, O2). The development of the sensors has been performed at the Institute for Micro- and Nanoelectronic, Technical University Ilmenau in co- operation with (GE) General Electric Global Research (USA) and Umwelt-Sensor- Technik GmbH (Geschwenda). Chapter 1: serves as an introduction into the scientific fields related to this work. The theoretical fundamentals of solid-state gas sensors are provided and the relevant properties of wide band gap materials (SiC and GaN) are summarized. In chapter 2: The performance of Pt/GaN Schottky diodes with different thickness of the catalytic metal were investigated as hydrogen gas detectors. The area as well as the thickness of the Pt were varied between 250 × 250 µm2 and 1000 × 1000 µm2, 8 and 40 nm, respectively. The response to hydrogen gas was investigated in dependence on the active area, the Pt thickness and the operating temperature for 1 vol.% hydrogen in synthetic air. We observed a significant increase of the sensitivity and a decrease of the response and recovery times by increasing the temperature of operation to about 350°C and by decreasing the Pt thickness down to 8 nm. Electron microscopy of the microstructure showed that the thinner platinum had a higher grain boundary density. The increase in sensitivity with decreasing Pt thickness points to the dissociation of molecular hydrogen on the surface, the diffusion of atomic hydrogen along the platinum grain boundaries and the adsorption of hydrogen at the Pt/GaN interface as a possible mechanism of sensing hydrogen by Schottky diodes. The response to deuterium D2, NOx, and O2 of metal-oxide-semiconductor (MOS) and metal-metal oxide-oxide-semiconductor (MMOOS) structures with rhodium (Rh) gate were investigated in dependence on the operating temperature and gas partial pressures was investigated in chapter 3. The response of the sensor was measured as a shift in the capacitance-voltge (C-V) curve along the voltage axis. Positive and negative flat-band voltage shifts up to 1 V were observed for oxidizing and reducing gases, respectively. Depending on the type of insulator that is chosen, differences in the sensitivity of the sensor were observed. IV Abstract In chapter 4: The performance of SiC-based field effect transistors (FETs) with different gate materials (mixture of metal oxides: indium oxide and tin oxide (InxSnyOz), indium oxide and vanadium oxide (InxVyOz), as well as mixtures of metal oxides with metal additives) were investigated as NOx, O2, and D2 gas detectors. The response to these gases was investigated in dependence on the operating temperature and gas partial pressures. The composition and microstructure of the sensing gate electrode are the key parameters that influence the sensing mechanism, and hence key performance parameters: sensitivity, selectivity, and response time. By choosing the appropriate temperature and catalyst material (gate material), devices that are significantly sensitive to certain gases may be realized. In addition, the temperature of maximum response varies dependent on the gas species being measured. This information, along with a careful choice of catalyst (gate material) can be used to enhance device selectivity. In chapter 5: Polycrystalline and nano-structured In2O3 thin films were investigated with the aim to obtain information about their NOx and O2 gas sensing properties. The response to these gases was investigated in dependence on the operating temperature and gas partial pressures. The analysis in the presence of different partial pressures of NOx has shown that both thin films are able to detect nitrogen oxide, but their responses exhibit different characteristics. In particular, nano-structured In2O3 thin films were found to have the higher response to NOx. This is most probably due to the enlarged overall active surface area of the sensing layer as a consequence of the small grain size (higher surface to volume ratio) so that the relative interactive surface area is larger, and the density of charged carriers per volume is higher. We have found that reducing the grain size of the sensing material to the ~10 nm regime can have a substantial effect on performance. The optimum detection temperatures of the nano-structured In2O3 occur in the range of 100-175°C for NOx considering the sensitivity as well as the response time. In this range of temperatures the response to O2 is very low indicating that the sensor is very suitable for selective detection of NOx at low temperatures In addition, nano-structured In2O3 thin films were found to be more suitable to be used in the field of application for detecting low partial pressures. Chapter 6: offers conclusions of the current work. In this chapter we compare also all studied gas sensors according to their sensitivity, selectivity, and response Abstract V time and then we compare them with the related works by other authors available in the scientific literature. VI Abstract Zusammenfassung VII Zusammenfassung Im Rahmen dieser Arbeit sind Feldeffektgassensoren (Schottky Dioden, MOS Kapazitäten, und MOSFET Transistoren) auf der Basis von Halbleitern mit großer Bandlücke (Siliziumkarbid (SiC) und Gallium Nitrid (GaN), sowie resistive Gassensoren, die auf aktiven Indiumoxid-Schichten (In2O3) basieren, für die Detektion von reduzierenden Gasen (H2, D2) und oxidierenden Gasen (NOx, O2), entwickelt worden. Die Entwicklung der Sensoren ist am Institut für Mikro- und Nanoelektronik der Technischen Universität Ilmenau in Zusammenarbeit mit General Electric (GE) Global Research (USA) und der Umwelt- und Sensortechnik GmbH (Geschwenda) durchgeführt worden. Kapitel 1: dient als eine Einführung in das mit dieser Arbeit verbundene wissenschaftliche Feld. Die theoretischen Grundlagen der Festkörper-Gassensoren werden dargestellt. Zusätzlich werden in diesem Kapitel die relevanten Eigenschaften der Materialien mit großer Bandlücke (SiC und GaN) präsentiert. Kapitel 2: Pt/GaN Schottky Dioden mit verschiedener Dicke des katalytischen Metalls werden als Wasserstoffgasdetektoren vorgestellt. Die Fläche sowie die Dicke von Pt-gates wurden zwischen 250 × 250 µm2 und 1000 × 1000 µm2, 8 und 40 nm, systematisch variiert. Die Sensorantwort (Sensorsreaktion) auf 1 vol.% Wasserstoff in synthetischer Luft wurde in Abhängigkeit von der aktiven Fläche, der Pt-Dicke, und der Betriebstemperatur untersucht. Durch Anheben der Betriebstemperatur auf ca. 350°C und durch Reduzierung der Dicke des Pt auf 8 nm beobachteten wir eine beträchtliche Erhöhung der Empfindlichkeit sowie eine Verkürzung der Ansprech- und Erholzeiten. Untersuchungen am Elektronenmikroskop zeigten, dass das dünnere Platin eine höhere Korngrenzendichte aufwies. Die Erhöhung der Empfindlichkeit gemeinsam mit der Reduzierung der Dicke des Pt deuten auf die Dissoziierung von molekularem Wasserstoff an der Oberfläche, die Diffusion atomaren Wasserstoffs entlang der Korngrenzen des Platins und die Adsorption von Wasserstoff an der Pt/GaN Grenzfläche als ein möglicher Mechanismus der Detektion von Wasserstoff durch Schottky Dioden hin. Die Reaktion auf D2, NOx, and O2 von Metall-Oxid-Halbleiter (MOS) Strukturen mit Rhodium Schottky-Kontakten mit einer Dicke von 30 nm in Abhängigkeit von der Betriebstemperatur und der Gaspartialdrücke wurde in Kapitel 3 untersucht. Die Reaktion dieses Gates wurde als Verschiebung entlang der Spannungsachse in der Kapazität-Spannungs Kurve (C-V) nachgewiesen. Positive und negative Flachband- VIII Zusammenfassung Verschiebungen jeweils bis zu 1 V wurden für oxidierende und reduzierende Gase beobachtet. Abhängig vom gewählten Typ des Isolators wurden Unterschiede in den Empfindlichkeiten beobachtet. In Kapitel 4: SiC-basierten FETs mit verschiedenen Materialien für das Gate (Gemisch aus Metalloxiden: Indiumoxide und Zinnoxid (InxSnyOz), Indiumoxid und Vanadiumoxid (InxVyOz) sowie ein Gemisch aus Metalloxiden mit Zugabe einer entsprechenden Menge Metallzusätzen) wurden als NOx, O2, und D2 Gasdetektoren untersucht. Die Reaktion auf diese Gase wurde in Abhängigkeit von der Betriebstemperatur und der Gaspartialdrücke untersucht. Die Zusammensetzung der aktiven Metalloxid-Schicht und die Mikrostruktur der sensitiven Gateelektrode sind die entscheidenden Parameter mit Einfluss auf den Messmechanismus und somit die entscheidenden Leistungsparameter des Sensors: Empfindlichkeit, Selektivität und Reaktionszeit. Durch die Optimierung der Temperatur und des richtigen Materials des Katalysators können Sensoren mit sehr hoher Empfindlichkeit
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