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The enabling technologies for the development of a flexible tag microlab for food monitoring during the logistic chain will be presented. The realisation of the system includes the integration of physical and chemical sensors with Radio Frequency IDentification (RFID) communication capabilities. The first ISO 15693 compliant semi-active tag prototype, including low power control electronics, RFID antenna, commercial sensors, memory and a thin film battery, is shown together with the development of novel ultra-low power hotplates required for this application and the process, based on the use of anisotropic conductive adhesive (ACA) flip chip technology, for gas sensors integration onto flexible substrates.

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In this work the development and optimization of the main components for a multisensing flexible Tag with RFID communication capabilities and integrated physical and chemical sensors for logistic datalogging applications will be reported. For this 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 ultralow-power Metal OXdide semiconductor (MOX) gas sensors 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, thus data acquisition and storage can be accomplished 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 front-end electronics, together with innovative ultralow-power MOX sensor arrays with flexible circuit encapsulation techniques will be described.

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.

In this paper, we investigated how different growth conditions (i.e., temperature, growth time, and composition) allows for trading off cost (i.e., In content) and performance of nanostructured indium tin oxide (ITO) for biosensing applications. Next, we compared the behavior of these functionalized nanostructured surfaces obtained in different growth conditions between each other and with a standard thin film as a reference, observing improvements in effective detection area up to two orders of magnitude. This enhanced the biosensor’s sensitivity, with higher detection level, better accuracy and higher reproducibility. Results show that below 150 °C, the growth of ITO over the substrate forms a homogenous layer without any kind of nanostructuration. In contrast, at temperatures higher than 150 °C, a two-phase temperature-dependent growth was observed. We concluded that (i) nanowire length grows exponentially with temperature (activation energy 356 meV) and leads to optimal conditions in terms of both electroactive surface area and sensitivity at around 300 °C, (ii) longer times of growth than 30 min lead to larger active areas and (iii) the In content in a nanostructured film can be reduced by 10%, obtaining performances equivalent to those found in commercial flat-film ITO electrodes. In summary, this work shows how to produce appropriate materials with optimized cost and performances for different applications in biosensing.

The electroactivity of nanostructured indium tin oxide (ITO) has been investigated for its further use in applications such as sensing biological compounds by the analysis of redox active molecules. ITO films were fabricated by using electron beam evaporation at different substrate temperatures and subsequently annealed for promoting their crystallization. The morphology of the deposited material was monitored by scanning electron microscopy, confirming the deposition of either thin films or nanowires, depending on the substrate temperature. Electrochemical surface characterization revealed a 45 % increase in the electroactive surface area of nanostructured ITO with respect to thin films, one third lower than the geometrical surface area variation determined by atomic force microscopy. ITO surfaces were functionalized with a model organic molecule known as 6-(ferrocenyl)hexanethiol. The chemical attachment was done by means of a glycidoxy compound containing a reactive epoxy group, the so-called 3-glycidoxypropyltrimethoxy-silane. ITO functionalization was useful for determining the benefits of nanostructuration on the surface coverage of active molecules. Compared to ITO thin films, an increase in the total peak height of 140 % was observed for as-deposited nanostructured electrodes, whereas the same measurement for annealed electrodes resulted in an increase of more than 400 %. These preliminary results demonstrate the ability of nanostructured ITO to increase the surface-to-volume ratio, conductivity and surface area functionalization, features that highly benefit the performance of biosensors.

Metal Oxide (MOX) gas sensors rely on chemical reactions that occur efficiently at high temperatures, resulting in too-demanding power requirements for certain applications. Operating the sensor under a Pulsed-Temperature Operation (PTO), by which the sensor heater is switched ON and OFF periodically, is a common practice to reduce the power consumption. However, the sensor performance is degraded as the OFF periods become larger. Other research works studied, generally, PTO schemes applying waveforms to the heater with time periods of seconds and duty cycles above 20%. Here, instead, we explore the behaviour of PTO sensors working under aggressive schemes, reaching power savings of 99% and beyond with respect to continuous heater stimulation. Using sensor sensitivity and the limit of detection, we evaluated four Ultra Low Power (ULP) sensors under different PTO schemes exposed to ammonia, ethylene, and acetaldehyde. Results show that it is possible to operate the sensors with total power consumption in the range of microwatts. Despite the aggressive power reduction, sensor sensitivity suffers only a moderate decline and the limit of detection may degrade up to a factor five. This is, however, gas-dependent and should be explored on a case-by-case basis since, for example, the same degradation has not been observed for ammonia. Finally, the run-in time, i.e., the time required to get a stable response immediately after switching on the sensor, increases when reducing the power consumption, from 10 minutes to values in the range of 10-20 hours for power consumptions smaller than 200 microwatts.