Temperature dependence and dynamic behaviour of full well capacity in pinned photodiode CMOS image sensors

This study presents an analytical model of the Full Well Capacity(FWC) in Pinned Photodiode (PPD) CMOS image sensors. By introducing the temperature dependence of the PPD pinning voltage, the existing model is extended (with respect to previous works) to take into account the effect of temperature on the FWC. It is shown, with the support of experimental data, that whereas in dark conditions the FWC increases with temperature, a decrease is observed if FWC measurements are performed under illumination. This study also shows that after a light pulse, the charge stored in the PPD drops as the PPD tends toward equilibrium. On the base of these observations, an analytical model of the dynamic behaviour of the FWC in non-continuous illumination conditions is proposed. The model is able to reproduce experimental data over six orders of magnitude of time. Both the static and dynamic models can be useful tools to correctly interpret FWC changes following design variations and to accurately define the operating conditions during device characterizations

Label-free detection of biomolecules with Ta2O5-based field effect devices

Dissertação para obtenção do Grau de Doutor em Nanotecnologias e NanociênciasInternational Iberian Nanotechnology Laboratory (INL

Developing ultrasensitive and CMOS compatible ISFETs in the BEOL of industrial UTBB FDSOI transistors

Le marché des capteurs a récemment connu une croissance spectaculaire alimentée par l'application remarquable de capteurs dans l'électronique de consommation, l'industrie de l'automatisation, les appareils portables, le secteur automobile et l'internet des objets de plus en plus adopté. La technologie avancée des complementary metal oxide semiconductor (CMOS), les technologies de nano et de micro-fabrication et les plateformes de synthèse de matériaux innovantes sont également des moteurs du développement incroyable de l'industrie des capteurs. Ces progrès ont permis la réalisation de capteurs dotés de nombreuses caractéristiques telles que la précision accrue, les dimensions miniaturisées, l’intégrabilité, la production de masse, le coût très réduit et le temps de réponse rapide. Les ion-sensitive field-effect transistors (ISFETs) sont des capteurs à l'état solide (bio) chimiques, destinés à la détection des ions H+ (pH), Na+ et K+. Malgré cela, la commercialisation des ISFETs est encore à ses balbutiements, après près de cinq décennies de recherche et développement. Cela est dû principalement à la sensibilité limitée, à la controverse sur l'utilisation de l'électrode de référence pour le fonctionnement des ISFETs et à des problèmes de stabilité. Dans cette thèse, les ISFETs ultrasensibles et compatibles CMOS sont intégrés dans le BEOL des transistors UTBB FDSOI standard. Un circuit diviseur capacitif est utilisé pour polariser la grille d’avant afin d'assurer des performances stables du capteur. En exploitant la fonction d’amplification intrinsèque fournie par les transistors UTBB FDSOI, nous avons présenté des ISFET ultra sensibles. L'amplification découle du fort couplage électrostatique entre la grille avant et la grille arrière du FDSOI et des capacités asymétriques des deux grilles. Un changement de tension au niveau de la grille avant apparaît sur la grille arrière sous la forme d'un décalage amplifié de la tension. L'amplification, représentée par le facteur de couplage (γ), est égale au rapport de la capacité de l'oxyde de grille et de la capacité de le buried oxide (BOX). Par conséquent, en fonctionnalisant la détection du pH sur la grille avant pour les dispositifs FDSOI, la modification du potentiel de surface sur la grille avant est détectée par la grille arrière et amplifiée du facteur de couplage (γ), donnant lieu à un capteur chimique à l'état solide à sensibilité ultra-élevée. L'intégration de la fonctionnalité de détection a été réalisée en back end of line (BEOL), ce qui offre les avantages d'une fiabilité et d'une durée de vie accrues du capteur, d'une compatibilité avec le processus CMOS standard et d'une possibilité d'intégration d'un circuit diviseur capacitif. Le fonctionnement des MOSFETs, sans une polarisation appropriée de la grille avant, les rend vulnérables aux effets de grilles flottantes indésirables. Le circuit diviseur capacitif résout ce problème en polarisant la grille avant tout enmaintenant la fonctionnalité de détection sur la même grille par un couplage capacitif au métal commun du BEOL. Par conséquent, le potentiel au niveau du métal BEOL est une somme pondérée du potentiel de surface au niveau de la grille de détection et de la polarisation appliquée au niveau de la grille de contrôle. Le capteur proposé est modélisé et simulé à l'aide de TCAD-Sentaurus. Un modèle mathématique complet a été développé. Il fournit la réponse du capteur en fonction du pH de la solution (entrée du capteur) et des paramètres de conception du circuit diviseur capacitif et du transistor UTBB FDSOI. Dans ce cas, des résultats cohérents ont été obtenus des travaux de modélisation et de simulation, avec une sensibilité attendue de 780 mV / pH correspondant à un film de détection ayant une réponse de Nernst. La modélisation et la simulation du capteur proposé ont également été validées par une fabrication et une caractérisation du capteur de pH à grille étendue avec validation de son concept. Ces capteurs ont été développés par un traitement séparé du composant de détection de pH, qui est connecté électriquement au transistor uniquement lors de la caractérisation du capteur. Ceci permet une réalisation plus rapide et plus simple du capteur sans avoir besoin de masques et de motifs par lithographie. Les capteurs à grille étendue ont présenté une sensibilité de 475 mV/pH, ce qui est supérieur aux ISFET de faible puissance de l'état de l’art. Enfin, l’intégration de la fonctionnalité de détection directement dans le BEOL des dispositifs FDSOI UTBB a été poursuivie. Une sensibilité expérimentale de 730 mV/pH a été obtenue, ce qui confirme le modèle mathématique et la réponse simulée. Cette valeur est 12 fois supérieure à la limite de Nernst et supérieure aux capteurs de l'état de l’art. Les capteurs sont également évalués pour la stabilité, la résolution, l'hystérésis et la dérive dans lesquels d'excellentes performances sont démontrées. Une nouvelle architecture de détection du pH est également démontrée avec succès, dans laquelle la détection est fonctionnalisée au niveau de la diode de protection de la grille plutôt que de la grille avant des dispositifs UTBB FDSOI. La commutation de courant abrupte, aussi basse que 9 mV/decade, pourrait potentiellement augmenter la sensibilité de polarisation fixée à 6,6 decade/pH. Nous avons démontré expérimentalement une sensibilité de 1,25 decade/pH supérieure à la sensibilité reportée à l’état de l’art.Abstract: The sensor market has recently seen a dramatic growth fueled by the remarkable application of sensors in the consumer electronics, automation industry, wearable devices, the automotive sector, and in the increasingly adopted internet of things (IoT). The advanced complementary metal oxide semiconductor (CMOS) technology, the nano and micro fabrication technologies, and the innovative material synthesis platforms are also driving forces for the incredible development of the sensor industry. These technological advancements have enabled realization of sensors with characteristic features of increased accuracy, miniaturized dimension, integrability, volume production, highly reduced cost, and fast response time. Ion-sensitive field-effect transistors (ISFETs) are solid state (bio)chemical sensors, for pH (H+), Na+, K+ ion detection, that are equipped with the promise of the highly aspired features of CMOS devices. Despite this, the commercialization of ISFETs is still at the stage of infancy after nearly five decades of research and development. This is due mainly to the limited sensitivity, the controversy over the use of the reference electrode for ISFET operation, and because of stability issues. In this thesis, ultrasensitive and CMOS compatible ISFETs are integrated in the back end of line (BEOL) of standard UTBB FDSOI transistors. A capacitive divider circuit is employed for biasing the front gate for stable performance of the sensor. Exploiting the intrinsic amplification feature provided by UTBB FDSOI transistors, we demonstrated ultrahigh sensitive ISFETs. The amplification arises from the strong electrostatic coupling between the front gate and the back gate of the FDSOI, and the asymmetric capacitances of the two gates. A change in voltage at the front gate appears at the back gate as an amplified shift in voltage. The amplification, referred to as the coupling factor (γ), is equal to the ratio of the gate oxide capacitance and the buried oxide (BOX) capacitance. Therefore, functionalizing the pH sensing at the front gate of FDSOI devices, the change in surface potential at the front gate is detected at the back gate amplified by the coupling factor (γ), giving rise to an ultrahigh-sensitive solid state chemical sensor. Integration of the sensing functionality was made in the BEOL which gives the benefits of increased reliability and life time of the sensor, compatibility with the standard CMOS process, and possibility for embedding a capacitive divider circuit. Operation of the MOSFETs without a proper front gate bias makes them vulnerable for undesired floating body effects. The capacitive divider circuit addresses these issues by biasing the front gate simultaneously with the sensing functionality at the same gate through capacitive coupling to a common BEOL metal. Therefore, the potential at the BEOL metal would be a weighted sum of the surface potential at the sensing gate and the applied bias at the control gate. The proposed sensor is modeled and simulated using TCAD-Sentaurus. A complete mathematical model is developed which provides the output of the sensor as a function of the solution pH (input to the sensor), and the design parameters of the capacitive divider circuit and the UTBB FDSOI transistor. In that case, consistent results have been obtained from the modeling and simulation works, with an expected sensitivity of 780 mV/pH corresponding to a sensing film having Nernst response. The modeling and simulation of the proposed sensor was further validated by a proof of concept extended gate pH sensor fabrication and characterization. These sensors were developed by a separated processing of just the pH sensing component, which is electrically connected to the transistor only during characterization of the sensor. This provides faster and simpler realization of the sensor without the need for masks and patterning by lithography. The extended gate sensors showed 475 mV/pH sensitivity which is superior to state of the art low power ISFETs. Finally, integration of the sensing functionality directly in the BEOL of the UTBB FDSOI devices was pursued. An experimental sensitivity of 730 mV/pH is obtained which is consistent with the mathematical model and the simulated response. This is more than 12-times higher than the Nernst limit, and superior to state of the art sensors. Sensors are also evaluated for stability, resolution, hysteresis, and drift in which excellent performances are demonstrated. A novel pH sensing architecture is also successfully demonstrated in which the detection is functionalized at the gate protection diode rather than the front gate of UTBB FDSOI devices. The abrupt current switching, as low as 9 mV/decade, has the potential to increase the fixed bias sensitivity to 6.6 decade/pH. We experimentally demonstrated a sensitivity of 1.25 decade/pH which is superior to the state of the art sensitivity

Field-Effect Sensors

This Special Issue focuses on fundamental and applied research on different types of field-effect chemical sensors and biosensors. The topics include device concepts for field-effect sensors, their modeling, and theory as well as fabrication strategies. Field-effect sensors for biomedical analysis, food control, environmental monitoring, and the recording of neuronal and cell-based signals are discussed, among other factors

Development of light-addressable potentiometric sensor systems and their applications in biotechnological environments

The simultaneous analysis of multiple analytes and spatially resolved measurements of concentration distributions with a single sensor chip are an important task in the field of (bio-)chemical sensing. Together with the miniaturisation, this is a promising step forward for applications and processes that profit from (bio-)chemical sensors. In combination with biological recognition elements, like enzymes or cells, these biosensors are becoming an interesting tool for e.g., biotechnological, medical and pharmaceutical applications. One promising sensor principle is the light-addressable potentiometric sensor (LAPS). A LAPS is a semiconductor-based potentiometric sensor that allows determining analyte concentrations of aqueous solutions in a spatially resolved manner. Therefore, it is using a focused light source to address the area of interest. The light that illuminates the local area of the LAPS chip generates a photocurrent that correlates with the local analyte concentration on the sensor surface. Based on the "state of the art", further developments of LAPS set-ups were carried out within this PhD thesis. Furthermore, by utilising enzymes and whole cells, the benefits of these LAPS set-ups for biotechnological, medical and pharmaceutical applications are demonstrated. During the present thesis, three different LAPS set-ups were developed: The first LAPS set-up makes use of a field-programmable gate array (FPGA) to drive a 4x4 light-emitting diode (LED) array that defines 16 measurement spots on the sensor-chip surface. With the help of the FPGA, the driving parameters, like light brightness, modulation amplitude and frequency can be selected individually and all LEDs can be driven concurrently. Thus, a simultaneous readout of all measurement spots is possible and chemical images of the whole sensor surface can be achieved within 200 ms. The FPGA-based LAPS set-up is used to observe the frequency behaviour of LAPS chips. In a second LAPS set-up, a commercially available organic-LED (OLED) display is used as light source. The OLED panel consists of 96x64 pixels with a pixel size of 200x200 µm and thus, an over 16 times higher lateral resolution compared to the IR-LED array. It was demonstrated that chemical images of the whole sensor surface can be obtained in 2.5 min. Since the lateral resolution of LAPS is not only specified by the light source, but also by the LAPS chip itself, the lateral resolution of the LAPS structures is characterised. Therefore, the third LAPS set-up has been developed, which utilises a single laser diode that can be moved by an XY-stage. By scanning a specially patterned LAPS chip, a lateral resolution of the LAPS structures in the range of the pixel size of the OLED display is demonstrated. Label-free imaging of biological phenomena is investigated with the FPGA-based LAPS. With the help of an enzymatic layer with the enzyme acetylcholine esterase (AChE) the detection of the neuronal transmitter acetylcholine (ACh) is demonstrated. The dynamic and static response as well as the long-term stability is characterised and compared with another semiconductor-based chemical imaging sensor based on charge-coupled devices (CCD) using the same enzymatic layer. The usage of the FPGA-based LAPS as whole-cell-based biosensor is studied with the model organism Escherichia coli. Here, the metabolic activity of the E. coli cells is investigated by determining the extracellular acidification. An immobilisation technique for embedding the microorganisms in polyacrylamide gel on the sensor surface has been developed. The immobilisation is realised in an on-chip differential arrangement by making use of the addressability of LAPS. This way, external influences such as sensor drift, temperature changes and external pH changes can be compensated. In a comparative study of the extracellular acidification rate between immobilised E. coli and E. coli that are in suspension, acidification rates in the same order were determined, demonstrating that the immobilisation does not have any influence on the metabolic activity. Further measurements with this cell-based LAPS system underline the sensitivity towards different nutrient concentrations, namely glucose. The ability to observe the extracellular acidification of microorganisms and the sensitively towards nutrient concentrations enables to detect high-order effects, like toxicity or pharmacological activity in complex analytes

Graphene inspired sensing devices

Graphene’s exciting characteristics such as high mechanical strength, tuneable electrical prop- erties, high thermal conductivity, elasticity, large surface-to-volume ratio, make it unique and attractive for a plethora of applications including gas and liquid sensing. Adsorption, the phys- ical bonding of molecules on solid surfaces, has huge impact on the electronic properties of graphene. We use this to develop gas sensing devices with faster response time by suspending graphene over large area (cm^2) on silicon nanowire arrays (SiNWAs). These are fabricated by two-step metal-assisted chemical etching (MACE) and using a home-developed polymer-assisted graphene transfer (PAGT) process. The advantage of suspending graphene is the removal of diffusion-limited access to the adsorption sites at the interface between graphene and its support. By modifying the Langmuir adsorption model and fitting the experimental response curves, we find faster response times for both ammonia and acetone vapours. The use of suspended graphene improved the overall response, based on speed and amplitude of response, by up to 750% on average. This device could find applications in biomedical breath analysis for diseases such lung cancer, asthma, kidney failure and more. Taking advantage of the mechanical strength of graphene and using the developed PAGT process, we transfer it on commercial (CMOS) Ion-Sensitive Field-Effect Transistor (ISFET) arrays. The deposition of graphene on the top sensing layer reduces drift that results from the surface modification during exposure to electrolyte while improving the overall performance by up to about 10^13 % and indicates that the ISFET can operate with metallic sensing membrane and not only with insulating materials as confirmed by depositing Au on the gate surface. Post- processing of the ISFET top surface by reactive ion plasma etching, proved that the physical location of trapped charge lies within the device structure. The process improved its overall performance by about 105 %. The post-processing of the ISFET could be applied for sensor performance in any of its applications including pH sensing for DNA sequencing and glucose monitoring.Open Acces

Laser direct written silicon nanowires for electronic and sensing applications

Silicon nanowires are promising building blocks for high-performance electronics and chemical/biological sensing devices due to their ultra-small body and high surface-to-volume ratios. However, the lack of the ability to assemble and position nanowires in a highly controlled manner still remains an obstacle to fully exploiting the substantial potential of nanowires. Here we demonstrate a one-step method to synthesize intrinsic and doped silicon nanowires for device applications. Sub-diffraction limited nanowires as thin as 60 nm are synthesized using laser direct writing in combination with chemical vapor deposition, which has the advantages of in-situ doping, catalyst-free growth, and precise control of position, orientation, and length. The synthesized nanowires have been fabricated into field effect transistors (FETs) and FET sensors. The FET sensors are employed to detect the proton concentration (pH) of an aqueous solution and highly sensitive pH sensing is demonstrated. Both top- and back-gated silicon nanowire FETs are demonstrated and electrically characterized. In addition, modulation-doped nanowires are synthesized by changing dopant gases during the nanowire growth. The axial p-n junction nanowires are electrically characterized to demonstrate the diode behavior and the transition between dopant levels are measured using Kelvin probe force microscopy

Chemical and biological sensors based on van der Waals heterostructures of graphene and carbon nanomembrane

In this thesis, single-layer graphene (SLG)-based field-effect devices were built to realize two different sensors: a pH sensor and a sensor measuring the concentration of the chemokine CXCL8 in clinical samples. CXCL8 is a signal protein that has various promising new applications in the field of disease diagnostics.20 For building these devices, a recently proposed new functionalization approach for graphene was employed.78 The approach is based on the assembly of an all-carbon van der Waals (vdW) heterostructure of carbon nanomembrane (CNM) and SLG. The effect of different substrates including SiO2, poly(ethylene 2,6-naphthalate) (PEN) and SiC and different types of SLG including graphene grown by chemical vapor deposition (CVD), epitaxial graphene, and nanoporous graphene (NPSLG) on the sensor response was investigated. Devices of increasing complexity were designed and investigated. At first, devices for measurements in vacuum. As a next step, devices for measurements of the pH value, and as final step the devices for biosensing. The fabrication of devices included their successive optimization based on transport measurements, electrical impedance spectroscopy (EIS) measurements, and surface sensitive characterization techniques. The device concept was the solution-gated field-effect transistor (SGFET),33 which has promising applications for point-of-care devices247 and lab-onchip technology