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Field-Effect Transistor Based Biosensing of Glucose Using Carbon

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Field-Effect Transistor Based Biosensing of Glucose Using Carbon Laboratoire d'Informatique, de Robotique et de Microelectronique´ de Montpellier Summer Internship 2019 Field-effect transistor based biosensing of glucose using carbon nanotubes and monolayer MoS2 Nathan Ullberg supervised by Aida Todri-Sanial examined by Carla Puglia November 24, 2019 Contents Abstract....................................2 Acknowledgements..............................3 1 Introduction..................................4 2 Background..................................5 2.1 Field-effect transistors (FET)....................5 2.1.1 Brief history and overview.................5 2.1.2 Characteristic curves....................6 2.1.3 Transconductance, threshold voltage, and ON/OFF ratio7 2.2 Field-effect biosensing (FEB)....................8 2.3 CNT-FETs.............................. 10 2.3.1 Dry CNT transistors.................... 10 2.3.2 Functionalization for glucose sensing........... 11 2.4 MoS2-FETs.............................. 12 2.4.1 Dry MoS2 transistors.................... 12 2.4.2 Biosensing applications................... 14 2.5 Graphene-FETs............................ 16 3 Results..................................... 17 3.1 CNT devices............................. 17 3.1.1 Fabrication......................... 17 3.1.2 SEM and AFM characterization.............. 19 3.1.3 Electrical characterization................. 22 3.2 MoS2 devices............................. 24 3.2.1 Fabrication......................... 24 3.2.2 Electrical characterization................. 25 4 Conclusions and next steps.......................... 26 Bibliography.................................. 32 Appendix I { Acronyms........................... 33 Appendix II { Procedure Guides....................... 34 1 Abstract As part of the EU SmartVista project to develop a multi-modal wearable sensor for health diagnostics, field-effect transistor (FET) based biosensors were explored, with glucose as the analyte, and carbon nanotubes (CNTs) or monolayer MoS2 as the semiconducting sensing layer. Numerous arrays of CNT-FETs and MoS2-FETs were fabricated by pho- tolithographic methods and packaged as integrated circuits. Functionalization of the sensing layer using linkers and enzymes was performed, and the samples were character- ized by atomic force microscopy, scanning electron microscopy, optical microscopy, and electrical measurements. ON/OFF ratios of 102 p-type and < 102 n-type were acheived, respectively, and the work helped survey the viability of realizing such sensors in a wear- able device. 2 Acknowledgements Firstly, I would like to thank my supervisor Dr Aida Todri-Sanial. She has been very supportive in ensuring that my internship experience is something meaningful both for myself and for the group. She has guided me and has helped sharpen my skills as a scientist. I have been working closely with post-doc Dr Abhishek Dahiya. His expertise, input, and patience have been invaluable to my internship experience. I also received much help from Dr Beno^ıtCharlot whose lab space and resources I was welcome to use, in addition to his advice, guidance, and help. I also thank post-doc Dr Marwa Dhifallah who helped me integrate into the environment and to understand the project, and Thierry Gil who provided help regarding electronics aspects. This internship was funded by the laboratory through my supervisor, as well as by a Eu- ropean Union (EU) Erasmus+ Student Mobility of Placement (SMP) grant (also known as a Traineeship). I therefore extend my thanks to the providers of these funds, which enabled me to focus on my work and to be less burdened by financial difficulties. I am also grateful for EU Horizon 2020, the eight Framework Program (FP8) since 1984 supporting research in the European Research Area, which is funding the SmartVista project.1,2 For this summer project I am also receiving 15 ECTS course credits, which contribute to my current Master's in Materials Physics program at Uppsala University. I am grateful to the program coordinator Professor Andreas Korn for his support and advice he has given me regarding my choices. I am also grateful to my home institution advisor Professor Carla Puglia; she evaluated my report and has been advising me in general regarding my academic choices. Finally I would like to thank my parents, sister, and friends for all their support. 3 1 Introduction The objective of this summer internship was to contribute in research and development concerning field-effect transistor (FET) based glucose sensing using carbon nanotubes (CNTs) and monolayer MoS2. This work is within the framework of the European Union Horizon 20203 project known as Smart Autonomous Multi Modal Sensors for Vital Signs Monitoring (SmartVista).1,2 The SmartVista project was launched in January 2019, and is a 3-year-long contract from the EU to help reduce deaths due to cardiovascular diseases (CVD) by a multi-modal wearable sensor. A schematic of the different modules in the wearable are shown in Figure 1. Figure 1: Modules in the SmartVista wearable. There are multiple partners from across Europe in this project working on the different modules. The partners include Tyndall National Institute (Ireland), University College Cork (Ireland), the French National Center for Scientific Research (CNRS) (France), NovoSense AB (Sweden), Fraunhofer { Research Institution for Microsystems and Solid State Technologies (EMFT) (Germany), and Analog Devices, Inc. (Ireland).1 The laboratory that I worked at is called The Montpellier Laboratory of Computer Sci- ence, Robotics, and Microelectronics (LIRMM) and is part of CNRS. The semiconduct- ing materials that were explored fall within a class of so-called 1D/2D materials, some of which include carbon nanotubes, graphene, and transition metal dichalcogenides (TMDs) like MoS2. These kinds of materials have attracted a lot of attention in the last two to three decades due to their various extraordinary and useful properties.4,5 For the internship the use of CNTs and monolayer MoS2 as the semiconducting chan- nel in the FET were explored for glucose sensing. Numerous arrays of CNT-FETs and MoS2-FETs were fabricated and characterized by electrical measurements, as well as by scanning electron microscopy (SEM), atomic force microscopy (AFM), and optical mi- croscopy. It should be noted that although the sensors were tested with different glucose molarities to detect changes in FET current, such measurements were not successful be- cause the devices were shorted by an ionic current or damaged during functionalization. Therefore for this report the data discussed will be regarding the quality of the sensors in \dry" conditions. The next section will be about the background, state of the art, and 4 mechanism for these kinds of sensors, followed by the results and data that were obtained, and finally a conclusion and discussion of the next steps for realizing these sensors. 2 Background 2.1 Field-effect transistors (FET) 2.1.1 Brief history and overview A transistor is a type of solid-state electronic device which conventionally is used in either switching or amplification applications. The former can be used for logical operations and therefore computing, while the latter is used for amplifying signals such as in a microphone. Before transistors, there were thermionic valves, also known as triodes or vacuum tubes which were used in computer processors such as in the 1945 ENIAC|the first electronic general-purpose computer. Vacuum tubes were problematic for several reasons however, such as that they consumed a lot of power and were not very stable. The solid-state transistor was superior, and was first fabricated at AT&T Bell Labs, New Jersey in 1947.6 The mechanism of a transistor is that it is a three-terminal device where a small input current or voltage controls a separate output current. The first 1947 transistor was a current-controlled point-contact transistor, of bipolar type, meaning both electrons and holes flow in the output current. What soon followed in 1948 was the invention of the bipolar junction transistor (BJT) which also is current-controlled and uses a more elegant junction approach of differently doped blocks of semiconductor connected by junctions. The first field-effect transistor was fabricated in 1953, and is a voltage-controlled transis- tor, where the electric field from the voltage causes charge to accumulate or deplete in the semiconductor and hence controls the output current. (FETs are unipolar meaning either electrons or holes flow in the channel but not both.) One way to think of such a device is as a voltage-controlled variable resistor.6,7 This is shown in Figure2. There are many different types of FETs, but the most common is a metal oxide semi- conductor FET (MOSFET), which was first fabricated in 1959. (More broadly these are called insulated-gate FETs (IGFETs) since the gate may not always be a metal and the dielectric may not always be an oxide.) As mentioned, MOSFETs are unipolar and hence can be either n-type (meaning electrons flow in the channel) or p-type (holes flow in the channel). The modes of a FET are either enhancement-mode (where the field causes carriers to accumulate) or depletion-mode (where the field depletes the channel of carri- ers). By very-large-scale integration (VLSI) of either n-type or p-type MOSFETs on a single chip (called NMOS and PMOS respectively), one can create a processor. However the most efficient approach is to use both, which is called complementary metal-oxide- semiconductor (CMOS) integration, which was invented in 1963. CMOS technology gave rise to the
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