Characterization of resistivity of Sb2S3 semiconductor nanowires by conductive AFM and in-situ methods

Conductive AFM and in situ methods were used to determine contact resistance and resistivity of individual Sb2S3 nanowires. Nanowires were deposited on oxidized Si surface for in situ measurements and on Si surface with macroelectrodes for conductive AFM (C-AFM) measurements. Contact resistance was determined by measurement of I(V) characteristics at different distances from the nanowire contact with the macroelectrode and resistivity of nanowires was determined. Sb2S3 is a soft material with low adhesion force to the surface and therefore special precautions were taken during measurements

Multiplexed DNA-Modified Electrodes

We report the use of silicon chips with 16 DNA-modified electrodes (DME chips) utilizing DNA-mediated charge transport for multiplexed detection of DNA and DNA-binding protein targets. Four DNA sequences were simultaneously distinguished on a single DME chip with 4-fold redundancy, including one incorporating a single base mismatch. These chips also enabled investigation of the sequence-specific activity of the restriction enzyme Alu1. DME chips supported dense DNA monolayer formation with high reproducibility, as confirmed by statistical comparison to commercially available rod electrodes. The working electrode areas on the chips were reduced to 10 μm in diameter, revealing microelectrode behavior that is beneficial for high sensitivity and rapid kinetic analysis. These results illustrate how DME chips facilitate sensitive and selective detection of DNA and DNA-binding protein targets in a robust and internally standardized multiplexed format

Biofilm dynamics characterization using a novel DO-MEA sensor: mass transport and biokinetics

Biodegradation process modeling is an essential tool for the optimization of biotechnologies related to gaseous pollutant treatment. In these technologies, the predominant role of biofilm, particularly under conditions of no mass transfer limitations, results in a need to determine what processes are occurring within the same. By measuring the interior of the biofilms, an increased knowledge of mass transport and biodegradation processes may be attained. This information is useful in order to develop more reliable models that take biofilm heterogeneity into account. In this study, a new methodology, based on a novel dissolved oxygen (DO) and mass transport microelectronic array (MEA) sensor, is presented in order to characterize a biofilm. Utilizing the MEA sensor, designed to obtain DO and diffusivity profiles with a single measurement, it was possible to obtain distributions of oxygen diffusivity and biokinetic parameters along a biofilm grown in a flat plate bioreactor (FPB). The results obtained for oxygen diffusivity, estimated from oxygenation profiles and direct measurements, revealed that changes in its distribution were reduced when increasing the liquid flow rate. It was also possible to observe the effect of biofilm heterogeneity through biokinetic parameters, estimated using the DO profiles. Biokinetic parameters, including maximum specific growth rate, the Monod half-saturation coefficient of oxygen, and the maintenance coefficient for oxygen which showed a marked variation across the biofilm, suggest that a tool that considers the heterogeneity of biofilms is essential for the optimization of biotechnologies.Peer ReviewedPostprint (published version

Electrochemical microsensors for cutaneous surface analysis: Application to the determination of pH and the antioxidant properties of stratum corneum

Potentiometry and cyclic voltammetry were proposed as simple, reliable and non invasive methods for the simultaneous determination of pH and antioxidant properties of skin. Experiments were performed with microelectrodes just deposited on skin surface without any gel or water added. pH was measured by means of the zero current potential of a tungsten W/WO3 sensor. A nerstian response was recorded in pH range 4 to 6 corresponding to the normal skin pH values. The global antioxidant capacity was deduced from the anodic charge passed during the plotting of cyclic voltammograms on platinum or gold microelectrodes. Comparing the half wave or peak potentials of these curves with those recorded for experiments performed in aqueous solution, the main hydrophilic antioxidants species were detected, i.e. ascorbic acid, uric acid and glutathione. This relatively easy-to-use analytical method made it possible to follow in real time the efficiency of topic treatment as well as to study the influence of oxidative stres

Usporedna procjena oksidacije amalgama kronopotenciometrijom i voltametrijom

The characteristic features of scanned deposition potential curves constructed from stripping chronopotentiometry (SSCP) and various modes of stripping voltammetry (SSV) are critically evaluated. The strengths and weaknesses of each method for identification of metal ion speciation features and susceptibility to typical interferences are described for conventional (HMDE) and microelectrodes, i.e. irreversibility in the electron transfer reaction, multi-metal resolution, intermetallic compound formation, homogeneous kinetics, induced metal adsorption, and requirement for excess ligand to avoid saturation at the electrode surface during reoxidation. The most advantageous stripping modes are those in which practically complete depletion of the accumulated metal is achieved during the reoxidation step, i.e. SCP with low stripping current and DC-SV with slow potential scan rate. Under these conditions there is a straightforward quantitative relationship between the amount of metal accumulated and the analytical signal. The slow rate of oxidation with these modes renders them practically immune to induced metal adsorption; they have a lower requirement for excess ligand in the sample solution and greater resistance to both irreversibility in the electrochemical oxidation and to interference from intermetallic compounds. Even in the case of nonreversible electrode processes, or for systems limited by complex formation/dissociation kinetics, depletive scanned deposition potential stripping curves allow complexation parameters to be determined from the shift in half-wave deposition potential, analogous to the DeFord-Hume approach for conventional voltammetry. SSCP has greater sensitivity, and provides greater resolution in multi-metal systems than does depletive DC-SSV, while SSV provides useful complementary information in some cases.Kritički su procijenjena karakteristična svojstva pseudopolarograma konstruiranih korištenjem dvaju metoda oksidacije amalgama: kronopotenciometrije i voltametrije. Pseudopolarogram je prikaz ovisnosti najvećeg intenziteta odziva oksidacije amalgama o potencijalu redukcije metalnih iona. Opisane su prednosti i mane obaju metoda pri određivanju raspodjele metalnih kompleksa i njihova podložnost tipičnim smetnjama. Analizirani su odzivi na visećoj živinoj kapi i na mikroelektrodama. Razmatrane su sljedeće pojave: reverzibilnost i brzina prijenosa elektrona, razdvajanje odziva većeg broja metala u živi, stvaranje intermetalnih spojeva u živi, utjecaji kemijskih reakcija koje prethode redukciji metalnih iona ili slijede oksidaciju amalgama, inducirana adsorpcija metalnih iona na površinu živine elektrode i minimalni višak slobodnog liganda potreban da se tijekom oksidacije amalgama svi metalni ioni uz površinu elektrode odmah kompleksiraju. Najbolja metoda oksidacije jest ona kojom se postiže potpuna oksidacija svih metalnih atoma akumuliranih u živi. Taj uvjet zadovoljavaju kronopotenciometrija sa slabom strujom i voltametrija sa sporom promjenom potencijala. Pod tim uvjetima postoji kvantitativna funkcionalna veza intenziteta odziva i količine akumuliranih metalnih atoma. Metode spore oksidacije su imune na induciranu adsorpciju, trebaju manji višak slobodnog liganda, manje ovise o brzini izmjene elektrona i manje im smetaju intermetalni spojevi. Ovim metodama mogu se odrediti konstante stabilnosti metalnih kompleksa i u slučajevima kinetički kontroliranih elektrodnih reakcija i sporih reakcija kompleksiranja ili disocijacije kompleksa. Pokazano je da je kronopotenciometrija osjetljivija od voltametrije i da se njenim korištenjem postiže bolja rezolucija odziva većeg broja metala, ali se voltametrijom mogu dobiti dodatne informacije o istraživanom sustavu

Neuronal Activity in the Human Subthalamic Nucleus Encodes Decision Conflict during Action Selection

The subthalamic nucleus (STN), which receives excitatory inputs from the cortex and has direct connections with the inhibitory pathways\ud of the basal ganglia, is well positioned to efficiently mediate action selection. Here, we use microelectrode recordings captured during\ud deep brain stimulation surgery as participants engage in a decision task to examine the role of the human STN in action selection. We\ud demonstrate that spiking activity in the STN increases when participants engage in a decision and that the level of spiking activity\ud increases with the degree of decision conflict. These data implicate the STN as an important mediator of action selection during decision\ud processes.\u

Fabrication and characterization of microfabricated on-chip microelectrochemical cell for biosensing applications

The fabrication of on-chip microelectrochemical cell on Si wafer by means of photolithography is described here. The single on-chip microelectrochemical cell device has dimensions of 100 × 380 mm with integrated Pt counter electrode (CE), Ag/AgCl reference electrode (RE) and gold microelectrode array of 500 nm recess depth as the working electrode (WE). Two geometries of electrode array were implemented, band and disc, with fixed diameter/width of 10 µm; and varied centre-to-centre spacing (d) and number of electrodes (N) in the array. The on-chip microelectrochemical cell structure has been designed to facilitate further WE biomodifications. Firstly, the developed microelectrochemical cell does not require packaging hence reducing the production cost and time. Secondly, the working electrode (WE) on the microelectrochemical cell is positioned towards the end of the chip enabling modification of the working electrode surface to be carried out for surface bio-functionalisation without affecting both the RE and CE surface conditions. The developed on-chip microelectrochemical cell was examined with scanning electron microscopy (SEM) and characterised by two electrochemical techniques. Both cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) were performed in 1 mM ferrocenecarboxylic acid (FCA) in 0.01 M phosphate buffered saline (PBS) solution at pH7.4. Electrochemical experiments showed that in the case of halving the interspacing distance of the microdisc WE array (50 nm instead of 100 nm), the voltammogram shifted from a steady-state CV (feature of hemispherical diffusion) to an inclined peak-shaped CV (feature of linear diffusion) albeit the arrays had the same surface area. In terms of EIS it was also found that linear diffusion dominates the surface instead of hemispherical diffusion once the interspacing distance was reduced, supporting the fact that closely packed arrays may behave like a macroelectrode

Synthesis and characterization of redox active cyrhetrene–triazole click products

We report the synthesis and characterization of two new cyclopentadienyl tricarbonyl rhenium(I) (cyrhetrene) complexes modified with a 1,4-disubstituted 1,2,3-triazole moiety. The two compounds, (η5-[4-phenyltriazol-1-yl]cyclopentadienyl) tricarbonyl rhenium(I), and (η5-[4-(4-aminophenyl)triazol-1-yl]cyclopentadienyl) tricarbonyl rhenium(I), were structurally characterized using 1H and 13C NMR, ATR-IR spectroscopy, UV–vis spectroscopy, mass spectrometry and X-ray crystallography where appropriate. The electrochemical behaviour of these two cyrhetrene–triazole complexes was explored using cyclic voltammetry, whereupon we observed that irreversible oxidation of the pendant 4-substituted-triazole moiety occurs before any electron transfer at the metal centre. This redox behaviour is in stark contrast to that of the analogous manganese(I) cymantrene–triazole derivatives, recently reported by our group

Chronic neural probe for simultaneous recording of single-unit, multi-unit, and local field potential activity from multiple brain sites

Drug resistant focal epilepsy can be treated by resecting the epileptic focus requiring a precise focus localization using stereoelectroencephalography (SEEG) probes. As commercial SEEG probes offer only a limited spatial resolution, probes of higher channel count and design freedom enabling the incorporation of macro and microelectrodes would help increasing spatial resolution and thus open new perspectives for investigating mechanisms underlying focal epilepsy and its treatment. This work describes a new fabrication process for SEEG probes with materials and dimensions similar to clinical probes enabling recording single neuron activity at high spatial resolution. Polyimide is used as a biocompatible flexible substrate into which platinum electrodes and leads are... The resulting probe features match those of clinically approved devices. Tests in saline solution confirmed the probe stability and functionality. Probes were implanted into the brain of one monkey (Macaca mulatta), trained to perform different motor tasks. Suitable configurations including up to 128 electrode sites allow the recording of task-related neuronal signals. Probes with 32 and 64 electrode sites were implanted in the posterior parietal cortex. Local field potentials and multi-unit activity were recorded as early as one hour after implantation. Stable single-unit activity was achieved for up to 26 days after implantation of a 64-channel probe. All recorded signals showed modulation during task execution. With the novel probes it is possible to record stable biologically relevant data over a time span exceeding the usual time needed for epileptic focus localization in human patients. This is the first time that single units are recorded along cylindrical polyimide probes chronically implanted 22 mm deep into the brain of a monkey, which suggests the potential usefulness of this probe for human applications