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The performance of transparent nanostructured indium tin oxide electrodes prepared by electron beam evaporation is optimized for biosensing purposes.

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.

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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.

Abstract:The development of miniaturized potentiostats capable of measuring in a wide range of conditions and with full characteristics (e.g., wide bandwidth and capacitive/inductive contribution to sensor's impedance) is still an unresolved challenge in bioelectronics. We present a simple analogue design coupled to a digital filter based on a lock-in amplifier as an alternative to complex architectures reported hitherto. A low-cost, miniaturized and fully integrated acquisition electronic system was developed, tested for a fully integrated three-lead electrochemical biosensor and benchmarked against a commercial potentiostat. The portable potentiostat was coupled to an array of miniaturized gold working electrodes to perform complex impedance analyses for tumor necrosis factor α (TNF-α) cytokine detection. This wearable potentiostat is very promising for the development of low-cost point-of-care (POC) with low power consumption.

Abstract:The need for miniaturized, low-cost and ultrasensitive electrochemical sensors has motivated the search and study of new nanostructured materials. We propose nanostructured indium tin oxide (ITO) electrodes as a promising platform due to their good electrical conductivity, transparency to visible wavelengths and high surface-to-volume ratio. The nanostructured electrodes were fabricated by electron beam evaporation, and electrochemical techniques were used to quantify more than a 40% increase in electrochemical surface area compared to thin ITO films. The electrodes were derivatized with organosilanes and coated with a molecule providing redox activity. Indeed, an increase in detectability of more than 400% was observed with respect to thin films, indicating the potential viability of nanostructured ITO-based electrochemical biosensors.