Une plate-forme sans fil pour electrochimique spectroscopie d'impédance

Avec l’émergence soutenue de capteurs et de dispositifs électrochimiques innovants, la spectroscopie d'impédance électrochimique est devenue l'un des outils les plus importants pour la caractérisation et la modélisation de la matière ionique et de l'interfaçage des capteurs. La capacité de détecter automatiquement, à l’aide de dispositifs électrochimiques peu couteux, les caractéristiques physiques et chimiques de la matière ionique ouvre une gamme d’application très variée pour la compréhension et l’optimisation des procédés ou interviennent les processus électrochimiques. Cette thèse décrit le développement d’une plate-forme microélectronique miniaturisée, connectée, multiplexée, et à faible coût pour la spectroscopie d'impédance diélectrique (SID) conçue pour les mesures électrochimiques in-situ et adaptée aux architectures de réseau sans fil. La plate-forme développée durant ce travail de maitrise a été testée et validée au sein d’une maille ZigBee et a été en mesure d'interfacer jusqu'à trois capteurs SID en même temps et de relayer l'information à travers le net Zigbee pour l'analyse de données et le stockage. Le système a été construit à partir de composants microélectroniques disponibles commercialement et bénéficie des avantages d'une calibration système on-the-fly qui effectue la calibration du capteur de manière aisée. Dans ce mémoire de maitrise, nous rapportons la modélisation et la caractérisation de senseurs électrochimiques de nitrate; notamment nous décrivons la conception microélectronique, la réponse d'impédance de Nyquist, la sensibilité et la précision de la mesure électrochimique, et les résultats de tests de la plate-forme pour les applications de spectroscopie d'impédance relatives à la détection du nitrate, de la détection de la qualité de l'eau, et des senseurs tactiles.The emergence of the various applications of electrochemical sensors and devices, electrochemical impedance spectroscopy became one of the most important tools for characterizing and modeling of the material and interfacing the sensors. The ability to sense in an automatic manner enables a wide variety of processes to be better understood and optimized cost-effectively. This thesis describes the development of a low-cost, miniaturized, multiplexed, and connected platform for dielectric impedance spectroscopy (DIS) designed for in-situ measurements and adapted to wireless network architectures. The platform has been tested and used as a DIS sensor node on a ZigBee mesh and was able to interface up to three DIS sensors at the same time and relay the information through the Zigbee net for data analysis and storage. The system was built from commercial microelectronics components and benefits from an on-the-fly calibration system that makes sensor calibration easy. The thesis reports characterizing and modeling of two electro-chemical devices (i.e. nitrate sensor and optically-transparent electrically-conductive glasses) and also describes the microelectronics design, the Nyquist impedance response, the measurement sensitivity and accuracy, and the testing of the platform for in-situ dielectric impedance spectroscopy applications pertaining to fertilizer sensing, water quality sensing, and touch sensing

Electrochemical Sensors and On-chip Optical Sensors

abstract: The microelectronics technology has seen a tremendous growth over the past sixty years. The advancements in microelectronics, which shows the capability of yielding highly reliable and reproducible structures, have made the mass production of integrated electronic components feasible. Miniaturized, low-cost, and accurate sensors became available due to the rise of the microelectronics industry. A variety of sensors are being used extensively in many portable applications. These sensors are promising not only in research area but also in daily routine applications. However, many sensing systems are relatively bulky, complicated, and expensive and main advantages of new sensors do not play an important role in practical applications. Many challenges arise due to intricacies for sensor packaging, especially operation in a solution environment. Additional problems emerge when interfacing sensors with external off-chip components. A large amount of research in the field of sensors has been focused on how to improve the system integration. This work presents new methods for the design, fabrication, and integration of sensor systems. This thesis addresses these challenges, for example, interfacing microelectronic system to a liquid environment and developing a new technique for impedimetric measurement. This work also shows a new design for on-chip optical sensor without any other extra components or post-processing.Dissertation/ThesisDoctoral Dissertation Electrical Engineering 201

Time Stamp – A Novel Time-to-Digital Demodulation Method for Bioimpedance Implant Applications

Bioimpedance analysis is a noninvasive and inexpensive technology used to investigate the electrical properties of biological tissues. The analysis requires demodulation to extract the real and imaginary parts of the impedance. Conventional systems use complex architectures such as I-Q demodulation. In this paper, a very simple alternative time-to-digital demodulation method or ‘time stamp’ is proposed. It employs only three comparators to identify or stamp in the time domain, the crossing points of the excitation signal, and the measured signal. In a CMOS proof of concept design, the accuracy of impedance magnitude and phase is 97.06% and 98.81% respectively over a bandwidth of 10 kHz to 500 kHz. The effect of fractional-N synthesis is analysed for the counter-based zero crossing phase detector obtaining a finer phase resolution (0.51˚ at 500 kHz) using a counter clock frequency ( fclk = 12.5 MHz). Because of its circuit simplicity and ease of transmitting the time stamps, the method is very suited to implantable devices requiring low area and power consumption

Online condition monitoring of lithium-ion and lead acid batteries for renewable energy applications

Electrochemical Impedance Spectroscopy (EIS) has been largely employed for the study of reaction kinetics and condition monitoring of batteries during different operational conditions, such as: Temperature, State of Charge (SoC) and State of Health (SoH) etc. The EIS plot translates to the impedance profile of a battery and is fitted to an Equivalent Electric Circuit (EEC) that model the physicochemical processes occurring in the batteries. To precisely monitor the condition of the batteries, Kramers-Kronig relation: linearity, stability and causality as well as the appropriate perturbation amplitude applied during EIS should be adhered to. Regardless of the accuracy of EIS, its lengthy acquisition time makes it impracticable for online measurement. Different broadband signals have been proposed in literature to shorten EIS measurement time, with different researchers favouring one technique over the other. Nonetheless, broadband signals applied to characterize a battery must be reasonably accurate, with little effect on the systems instrumentation. The major objective of this study is to explore the differences in the internal chemistries of the lithium-ion and lead acid batteries and to reduce the time associated with their condition monitoring using EIS. In this regard, this study firstly queries the methodology for EIS experiments, by investigating the optimum perturbation amplitude for EIS measurement on both the lead acid and lithium-ion batteries. Secondly, this study utilizes electrochemical equations to predict the dynamics and operational conditions associated with batteries. It also investigates the effect of different operational conditions on the lead acid and lithium-ion batteries after EEC parameters have been extracted from EIS measurements. Furthermore, different broadband excitation techniques for rapid diagnostics are explored. An online condition monitoring system is implemented through the utilization of a DC-DC converter that is used to interface the battery with the load. The online system is applied alongside the different broadband signals. The deviation in the broadband impedance spectroscopy result is compared against the Frequency Response Analyzer (FRA) to determine the most suitable technique for battery state estimation. Based on the comparisons, the adoption of a novel technique – Chirp Broadband Signal Excitation (CBSE) is proposed for online condition monitoring of batteries, as it has the advantage of being faster and precise at the most important frequency decade of the impedance spectrum of batteries

A Goertzel Filter Based System for Fast Simultaneous Multi-Frequency EIS

Bioimpedance measurement is a non-invasive, radiation-free, and inexpensive method for measuring the electrical properties of biological tissues. In applications where transients occur, the commonly used swept sinewave is replaced with broadband signals such as multisine. This makes the signal generation and the extraction of the real and imaginary parts of the impedance challenging. In this brief, an alternative to traditional fast Fourier transform (FFT) or coherent demodulation is presented. Based on the Goertzel filter, this alternative is simpler and requires very few digital resources. Its robustness to the harmonic fold back phenomenon, enables simple ternary current pulses to be used for excitation. The developed digital architecture is capable of simultaneous demodulation of 16 frequencies with an accuracy of 97% and 96% on the magnitude and phase measurement respectively. Employing a ternary sequence allows the use of a low power H-bridge current driver. The analog front-end and demodulation algorithm were implemented in an ASIC using a 180-nm CMOS technology. The system was tested on an isolated pig heart distinguishing edema from non-edema tissue by impedance changes

Bioimpedance Technique for Point-of-Care Devices Relying on Disposable Label-Free Sensors – An Anemia Detection Case

In this chapter, the development of a point-of-care device for bio-medical applications has been discussed. Our main objective is to research new electronic solutions for the detection, quantification, and monitoring of important biological agents in medical environments. The proposed systems and technologies rely on label-free disposable sensors, with portable electronics for user-friendly, low-cost solutions for medical disease diagnosis, monitoring, and treatment. In this chapter, we will focus on a specific point-of-care device for cellular analysis, applied to the case of anemia detection and monitoring. The methodology used for anemia monitoring is based on hematocrit measurement directly from whole blood samples by means of impedance analysis. The designed device is based on straightforward electronic standards for low power consumption and low-cost disposable sensor for low volume samples, resulting in a robust and low power consumption device for portable monitoring purposes of anemia. The device has been validated through different whole blood samples to prove the response, effectiveness, and robustness to detect anemia

Crexens™: an expandable general-purpose electrochemical analyzer

2019 Fall.Includes bibliographical references.Electrochemical analysis has gained a great deal of attention of late due to its low-cost, easy-to-perform, and easy-to-miniaturize, especially in personal health care where accuracy and mobility are key factors to bring diagnostics to patients. According to data from Centers for Medicare & Medicaid Services (CMS) in the US, the share of health expenditure in the US has been kept growing in the past 3 decades and reached 17.9% of its overall Gross Domestic Product till 2016, which is equivalent to $10,348 for every person in the US per year. On the other hand, health care resources are often limited not only in rural area but also appeared in well-developed countries. The urgent need and the lack of health resource brings to front the research interest of Point-of-Care (PoC) diagnosis devices. Electrochemical methods have been largely adopted by chemist and biologist for their research purposes. However, several issues exist within current commercial benchtop instruments for electrochemical measurement. First of all, the current commercial instruments are usually bulky and do not have handheld feature for point-of-care applications and the cost are easily near$5,000 each or above. Secondly, most of the instruments do not have good integration level that can perform different types of electrochemical measurements for different applications. The last but not the least, the existing generic benchtops instruments for electrochemical measurements have complex operational procedures that require users to have a sufficient biochemistry and electrochemistry background to operate them correctly. The proposed Crexens™ analyzer platform is aimed to present an affordable electrochemical analyzerwhile achieving comparable performance to the existing commercial instruments, thus, making general electrochemical measurement applications accessible to general public. In this dissertation, the overall Crexens™ electrochemical analyzer architecture and its evolution are presented. The foundation of the Crexens™ architecture was derived from two separate but related research in electrochemical sensing. One of them is a microelectrode sensor array using CMOS for neurotransmitter sensing; the other one is a DNA affinity-based capacitive sensor for infectious disease, such as ZIKA. The CMOS microelectrode sensor array achieved a 320uM sensitivity for norepinephrine, whereas the capacitive sensor achieved a dynamic range of detection from 1 /uL to 105 /uL target molecules (20 to 2 million targets), which makes it be within the detection range in a typical clinical application environment. This dissertation also covers the design details of the CMOS microelectrode array sensor and the capacitive sensor design as a prelude to the development of the Crexens™ analyzer architecture. Finally, an expandable integrated electrochemical analyzer architecture (Crexens™) has been designed for mobile point-of-care (POC) applications. Electrochemical methods have been explored in detecting various bio-molecules such as glucose, lactate, protein, DNA, neurotransmitter, steroid hormone, which resulted in good sensitivity and selectivity. The proposed system is capable of running electrochemical experiments including cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS), electrochemical capacitive spectroscopy (ECS), amperometry, potentiometry, and other derived electrochemical based tests. This system consist of a front-end interface to sensor electrodes, a back-end user interface on smart phone and PC, a base unit as master module, a low-noise add-on module, a high-speed add-on module, and a multi-channel add-on module. The architecture allows LEGO™-like capability to stack add-on modules on to the base-unit for performance enhancements in noise, speed or parallelism. The analyzer is capable of performing up to 1900 V/s CV with 10 mV step, up to 12 kHz EIS scan range and a limit of detection at 637 pA for amperometric applications with the base module. With high performance module, the EIS scan range can be extended upto 5 MHz. The limit of detection can be further improved to be at 333 fA using the low-noise module. The form factor of the electrochemical analyzer is designed for its mobile/point-of-care applications, integrating its entire functionality on to a 70 cm² area of surface space. A glutamine enzymatic sensor was used to valid the capability of the proposed electrochemical analyzer and turned out to give good linearity and reached a limit of detection at 50 uM

Integrated impedance spectroscopy biosensors

textAffinity-based biosensors, or in short biosensors, are extremely powerful and versatile analytical tools which are used for the detection of a wide variety of bio-molecules. In recent times, there has been a need for developing low-cost and portable affinity-based biosensor platforms. Such systems need to have a high density of detection sites (i.e biosensing elements) in order to simultaneously detect multiple analytes in a single sample. This has led to the creation of integrated biosensors, which make use of integrated circuits (ICs) for bio-molecular detection. In such systems, it has been demonstrated that by taking advantage of the capabilities of semiconductor and very large scale integrated (VLSI) circuit fabrication processes, it is possible to build compact miniaturized biosensors, which can be used in wide variety of applications such as in molecular diagnostics and for environmental monitoring. Among the various detection modalities for biosensors, Electrochemical Impedance Spectroscopy (EIS) permits real-time detection and has label-free detection capabilities. EIS is fully electronic in nature. Hence, it can be implemented using standard IC technologies. The versatility and ease of integration of EIS makes it a promising candidate for developing integrated biosensor platforms. In this thesis, we first examine the underlying principles of EIS method of biosensing. By analyzing an immunosensor assay as an example, we show that EIS based biosensing is a highly sensitive detection method, which can be used for the detection of a wide variety of analytes. Since EIS relies on small impedance changes in order to perform detection, it requires highly accurate models for the electrode-electrolyte systems. Hence, we also introduce a compact modeling technique for the distributed electrode-electrolyte systems with non-uniform electric fields, which is capable of modelling noise and other non-idealities in EIS. In the second part of this thesis, we describe the design and implementation of an integrated EIS biosensor array, built using a standard complementary metal-oxide-semiconductor (CMOS) process. The chip is capable of measuring admittance values as small as 10nS and has a wide dynamic range (90dB) over a wide range of frequencies (10Hz-50MHz). We also report the results obtained from the DNA and protein detection experiments performed using this chip.Electrical and Computer Engineerin