Francisco Palacio

Organosilane-functionalization of nanostructured indium tin oxide films

Fabrication and organosilane-functionalization and characterization of nanostructured ITO electrodes are reported. Nanostructured ITO electrodes were obtained by electron beam evaporation, and a subsequent annealing treatment was selectively performed to modify their crystalline state. An increase in geometrical surface area in comparison with thin-film electrodes area was observed by atomic force microscopy, implying higher electroactive surface area for nanostructured ITO electrodes and thus higher detection levels. To investigate the increase in detectability, chemical organosilane-functionalization of nanostructured ITO electrodes was performed. The formation of 3-glycidoxypropyltrimethoxysilane (GOPTS) layers was detected by X-ray photoelectron spectroscopy. As an indirect method to confirm the presence of organosilane molecules on the ITO substrates, cyclic voltammetry and electrochemical impedance spectroscopy (EIS) were also carried out. Cyclic voltammograms of functionalized ITO electrodes presented lower reduction-oxidation peak currents compared with non-functionalized ITO electrodes. These results demonstrate the presence of the epoxysilane coating on the ITO surface. EIS showed that organosilane-functionalized electrodes present higher polarization resistance, acting as an electronic barrier for the electron transfer between the conductive solution and the ITO electrode. The results of these electrochemical measurements, together with the significant difference in the X-ray spectra between bare ITO and organosilane-functionalized ITO substrates, may point to a new exploitable oxide-based nanostructured material for biosensing applications. As a first step towards sensing, rapid functionalization of such substrates and their application to electrochemical analysis is tested in this work. Interestingly, oxide-based materials are highly integrable with the silicon chip technology, which would permit the easy adaptation of such sensors into lab-on-a-chip configurations, providing benefits such as reduced size and weight to facilitate on-chip integration, and leading to low-cost mass production of microanalysis systems.

A low-cost and miniaturized potentiostat for sensing of biomolecular species such as TNF-α by electrochemical impedance spectroscopy

Miniaturizing potentiostats, keeping their cost low and yet preserving full measurement characteristics (e.g. bandwidth, determination of capacitive/inductive contribution to sensors impedance and parallel screening) is still an unresolved challenge in bioelectronics. In this work, the combination of simple analogue circuitry together with powerful microcontrollers and a digital filter implementation is presented as an alternative to complex and incomplete architectures reported in the literature. A low-cost acquisition electronic system fully integrated with a biosensors platform containing eight gold working microelectrodes and integrated reference and counter electrodes was developed and validated. The manufacturing cost of the prototype was kept below 300 USD. The performance of the proposed device was benchmarked against a commercial impedance analyzer through the electrochemical analysis of a highly sensitive biosensor for the detection of tumor necrosis factor α (TNF-α) within the randomly chosen range of 266pg/mL to 666ng/mL in physiological medium (PBS). A strong correlation between the outputs of both devices was found in a critical range of frequencies (1-10Hz), and several TNF-α cytokine concentrations were properly discriminated. These results are very promising for the development of low-cost, portable and miniaturized electrochemical systems for point-of-care and environmental diagnosis.

Ultra-low-power electronics and devices for a multisensing RFID Tag

A multisensing flexible Tag microlab (FTM) with RFID communication capabilities and integrated physical and chemical sensors for logistic datalogging applications is being developed. For this very specific scenario, several constraints must be considered: power consumption must be limited for long-term operation, reliable ISO compliant RFID communication must be implemented, and special encapsulation issues must be faced for reliable sensor integration. In this work, the developments on application specific electronic interfaces and on ultra-low-power MOX gas sensors in the framework of the GoodFood FP6 Integrated Project will be reported. The electronics for sensor control and readout as well as for RFID communication are based on an ultra-low-power MSP430 microcontroller from Texas Instruments together with a custom RFID front-end based on analog circuitry and a CPLD digital device, and are designed to guarantee a passive ISO15693 compliant RFID communication in a range up to 6 cm. A thin film battery for sensor operation is included, allowing data acquisition and storage when no reader field is present. This design allows the user to access both the traceability and sensor information even when the on-board battery is exhausted. The physical sensors for light, temperature and humidity are commercially available devices, while for chemical gas sensing innovative MOX sensors are developed, based on ultra-low-power micromachined hotplate arrays specifically designed for flexible Tag integration purposes. A single MOX sensor requires only 8.9 mW for continuous operation, while temperature modulation and discontinuous sensor operation modes are implemented to further reduce the overall power consumption. The development of the custom control and RFID electronics, together with innovative ultra-low-power MOX sensor arrays with flexible circuit encapsulation techniques will be reported in this work.

Evaluation of MOX Sensor Characteristics in Ultra-Low Power Operation Modes: Application to a Semi-Passive RFID Tag for Food Logistics

Most of the battery powered systems with integrated sensors need low power consumption modes to enlarge the operation time. In the case of the fruit logistic chain, the fruit quality may be controlled by the detection of some gases as ethylene, acetaldehyde and ammonia, that are related to maturation, oxygen stress and refrigeration leakage. We report the integration of an ultra-low power (ULP) metal oxide (MOX) sensor array inside a Radio Frequency IDentification (RFID) 13.56 MHz ISO/IEC 15693 compliant tag with temperature, humidity and light sensors and data logging capabilities. Pulsed Temperature Operation (PTO), which consists in switching on and off the sensor heater, was used to reduce power consumption more than three orders of magnitude, from 14 mW down to 7 μW. The sensor behavior was characterized in terms sensitivity for ammonia.