Semiconducting hexathiapentacene (HTP) single–crystal nanowires were synthesized using a simple solution-phase route. Quartz Crystal Microbalance and complex resistance measurements were employed to investigate the sensing properties of an HTP nanowire to analytes including acid, amine, and hydrocarbon vapors. Cole-Cole plots (0.01Hz-4 MHz) of measured impedance spectra, modeled using equivalent circuits, were used to resolve the effects of adsorption and charge migration.

Silver nanoparticles coated by a layer of gold (Ag@Au) have received much attention because of their potential application as ultra sensitive probes for the detection of biologically important molecules such as DNA, proteins, amino acids and many others. However, the ability to control the size, shape, and monodispersity of the Ag@Au structure has met with limited success. In our own research we have addressed this challenge by creating an aqueous wet chemical synthesis technique towards size and shape controllable Ag@Au nanoparticles. These materials are highly interesting because of the tunable silver core size, and the tunable gold shell thickness, opening many avenues to the modification of the particle properties in terms of bio-molecular sensing. The resulting nanoparticle probes were functionalized with two complementary stranded DNA oligonucleotides. When combined, the complementary strands hybridized, causing the Ag@Au nanoparticles to assemble into large nano-structures. The presence of the oligonucleotide was confirmed through a series of techniques including UV-Vis and RAMAN spectroscopy, as well as HR-TEM, XPS, DLS, and many others. The results reflect the role that the nanoparticle physical properties play in the detection of the bio-molecules, as well as elucidate the characteristics of the bio-molecule/nanoparticle interaction.

The first paper showing the great potentiality of Carbon Nanotubes Field Effect transistors (CNTFETs) for gas sensing applications was published in 2000 [1]. It has been demonstrated that the performances of this kind of sensors are extremely interesting : a sensitivity of around 100ppt (e.g. for NO2 [2]) has been achieved in 2003 and several techniques to improve selectivity have been tested with very promising results [2]. The main issues that have not allowed, up to now, these devices to strike more largely the market of sensors, have been the lack of an industrial method to obtain low-cost devices, a demonstration of their selectivity in relevant environments and finally a deeper study on the effect of humidity and the possible solutions to reduce it. This contribution deals with CNTFETs based sensors fabricated using air-brush technique deposition on large surfaces. Compared to our last contribution [3], we have optimized the air-brush technique in order to obtain high performances transistors (Log(Ion)/ Log(Ioff) ~ 5/6) with highly reproducible characteristics : this is a key point for the industrial exploitation. We have developed a machine which allows us the dynamic deposition on heated substrates of the SWCNT solutions, improving dramatically the uniformity of the SWCNT mats. We have performed tests using different solvents that could be adapted as a function of the substrates (e.g. flexible substrates). Moreover these transistors have been achieved using different metal electrodes (patented approach [4]) in order to improve selectivity. Results of tests using NO2, NH3 with concentrations between ~ 1ppm and 10ppm will be shown during the meeting.

Long-ranged double layer interactions and specific tip penetration through the scanned layers should be considered when atomic force microscopy (AFM) is used to probe soft samples such as surfactants or biological material within liquid media. Therefore, AFM imaging of soft nanostructures requires a careful adjust of the applied force and the scanning velocity. A paramount advantage of this technique is that cells immersed in liquids can be imaged under physiological conditions. On the other hand, confocal Raman microscopy (CRM) allows the real-time monitoring and chemical characterization of compounds also in a noncontact manner. The three-dimensional distribution of substances can be recorded by CRM with high spatial resolution by scanning a tightly focused laser beam over the sample. By combining of these two techniques (AFM and CRM), it is possible to obtain relevant information on formation processes, characteristics and behavior of soft self-assembled nanostructures and of cells on hydrophilic or hydrophobic surfaces under physiological conditions.

Rapidly responding, reversible, sensitive, and selective porous silicon-based (PS) gas sensors, operating at low power, are formed with a highly efficient electrical contact to a nanopore covered microporous array. Significant changes in sensor surface sensitivity can be correlated with the strong and weak acid-base (HSAB) character of the interacting gas analyte and the acidic nature of the PS surface so as to produce a dominant physisorption and create a range of highly selective surface coatings. This selection process dictates the application of nanostructured metal oxide and/or nanoparticle catalytic coatings, and provide for notably higher sensitivities which, in concert, form a basis for selectivity. Depositions which include AuxO, SnOx (Sn+2,+4) , CuxO ( Cu+1,+2), NiO(Ni+2) , nano-alumina, and titania, provide for the detection of gases including NO, NO2, CO, NH3, PH3, and H2S in an array-based format at the sub-ppm level. The value of this conductometric sensor technology results from a combination of (1) its sensitivity and short recovery time, (2) its operation at room temperature as well as at a single, readily accessible, temperature with an insensitivity to temperature drift, (3) its potential operation in a heat-sunk configuration allowing operation to a surface temperature of 80°C even in highly elevated temperature environments (in sharp contrast to metal oxide sensors), (4) its ease of coating with diversity of clearly mapped gas-selective materials for form sensor arrays, (5) its low cost of fabrication and operation, (6) its low power consumption, (7) its ease of rejuvenation following contamination, and (8) its ability to rapidly assess false positives using FFT techniques, operating the sensor in a pulsed gas mode.

Nanopore covered microporous silicon conductometric gas sensors have been produced via electrochemical etching and standard microfabrication techniques. Reversible and sensitive gas sensors working at room temperature have been fabricated. Sensing of NH3, NOx and PH3 at or below the ppm level have been achieved. The porous silicon (PS) surface has been modified using selective coatings including electroless tin, gold, nickel and copper solutions to increase the response to NOx, NH3, and PH3 respectively. The diffusion of the analyte species has been investigated in the nanopore and micropore regimes by numerical analysis. Comparing the response time of the hybrid porous sensor surface with numerical diffusion calculations on the pores, it has been observed that Knudsen diffusion time scales dominate the sensor response. A transduction model is proposed based on nanopore limited gas diffusion and the experimental response and recovery data.

We show a novel route to prepare SERS substrates, which is based on polymer–metal nanocomposites with a specific structure and composition just below the percolation threshold. The neighboring nanoparticles are still quite densely packed, but remain separated by narrow polymer gaps (<1 nm). Such a nanostructure allows the creation of densely packed hot spots where electromagnetic energy can be confined. The polymer–metal nanocomposites are fabricated by a simple and single-step method of electron-beam-assisted vapor-phase co-deposition. The preparation of the SERS substrates is based on a simple plasma-etching process, which removes the polymer structures that allow the formation of metal nanoparticle SERS nano-aggregates with very uniform and controllable inter-particle gaps. The method results in “ideal SERS hot spots” throughout the matrix. These hot spots can be created over very large areas. The prepared SERS substrates are promising candidates for the direct detection (label-free) and analysis of various biological and chemical samples.

In this work, the drift of ISFET characteristics due to hydration effect was studied. The ISFETs were fabricated using the standard NMOS process. The AgCl reference electrode was fabricated with the electrolysis method. The ISFET modeling was carried out in MATLAB to study the time variation of surface potential and the drain-source current. In addition, the surface morphology and dielectric constant of silicon dioxide were tested to study the hydration effect in order to eliminate the drift. The dielectric constant of the gate oxide increases exponentially with hydration time. The surface morphology studied with the atomic force microscope (AFM) showed no significant change after immersion in water. It is believed that the main cause of the drift is the hydration effect, which is due to the change in dielectric constant of the sensing material and a small number of surface binding sites that react slowly to a change in pH.

Surface plasmon resonance (SPR) biosensors are widely used in sensitive chemical, biological and environmental sensing. Recently, the studies of nano-plasmonics in metallic structures have shown that surface plasmons can also be excited by the metallic nanostructures films which can be used for high-throughput and chip-based SPR type sensing. We developed a class of plasmonic crystal-like structures consisting of a film with arrays of periodic nanoslit geometry. Because the engineered array ensures multiple resonance modes, we use the multispectral analysis to evaluate the refractive index sensing capability. Different from the common method monitoring a single peak shift, the multispectral analysis, observing all the peak shifts and intensity changes in the multiple plasmonic resonances in the spectra, can improve the signal-to-noise ratio of the system and enhance the sensing capabilities. In this investigation, we studied the best condition for the gold nanoslit arrays by testing their ability for refractive index sensing, and a high sensitivity of up to 28586 %T nm/RIU was obtained by multispectral analysis (RIU = refreactive index unit, and T= transmission).

Highly Focused Ion Beams (FIB) are used to produce in one step large quantities of solid state nanopores drilled in thin dielectric films with high reproducibility and well controlled morphologies. We explore both the production of nanopores of various diameters and study their applicability to different biological molecules such as DNA, or folded and unfolded proteins, and then we compare their transport properties. We also report on the translocation of Fibronectin which an original experiment made possible is using the methodology described in this article.

Magnetoelastic (ME) sensors provide a fast, sensitive method to detect bacteria with smaller sensors have higher mass sensitivity for detecting lower concentrations of bacteria. However, signals from smaller sensors are weaker and have more noise due to manufacturing defects. In this paper, we present a biosensor system for the detection of Salmonella typhimurium using multiple magnetoelastic sensors, each with the size of 2000 × 400 × 30 μm. The sensors are immobilized with E2 phage, which specifically binds with S. typhimurium. Unlike traditional methods, our system uses a step pulse to “shock” the sensor, causing it to vibrate at its natural resonance frequency and produce a signal in the pickup coil due to reverse magnetostriction. A Fast Fourier Transform (FFT) was used to determine the resonance frequency. As the biosensor captures S. typhimurium cells, its mass increases with a corresponding decrease of its resonance frequency.The detection system was composed of one coil with a reference sensor to monitor stability, and another coil with three measurement sensors separated in three tubes for simultaneous detection of bacteria. With multi-sensors the effect of a manufacturing defect is decreased and we get the benefit of averaging for more accurate and reliable results. Stability tests show that the variance of frequency detection is less than 122 ppm of its resonance frequency. SEM pictures of the sensor surface show a uniform binding of S. typhimurium cells. Cells were counted and the mass change calculated. The measured frequency change corresponds well to the theoretical change. The results show that the multiple phage based ME biosensors are able to simultaneously detect S. typhimurium and offer good sensitivity and reliability of detection.

A robust silicon gas sensor chip (platinum heater, low deformation membrane) has been designed and successfully operated with various metal oxide nanoparticles synthesized by an organometallic route (SnO2, ZnO) and deposited by a generic ink-jet method. High quality and micron thick layers are obtained and the CO gas sensitivity is presented.

Alkylene-bridged hybrid glass doped with Cr/CrOx was developed by sol-gel polymerization. When laser beam goes through a solid media, density wave is linear since heat doesn't decay through the media effectively in solid media. Interestingly, we observed a strong ‘acoustic response' from alkylene-bridged hybrid glass doped with Cr/CrOx due to high grating effect, high photo acoustic diffraction efficiency. The acoustic response generated from the doped hybrid glass was as compressive as liquid thus the acoustic refractive intensity generated from the hybrid glass was as strong as liquid. In our laser experiment, the diffraction efficiency (45%) of the glass is higher than that of methanol (25%). The hybrid glass can be used to develop diffraction beam modulators.

Plants, when attacked by herbivores emit plant volatile compounds as a defensive mechanism to protect themselves from herbivores and parasites. Secreting these volatiles is not only toxic towards these insects but also aids enemies of the herbivores to recognize infested plants to locate their prey. A low mass fraction carbon black/polyethylene-co-vinylacetate composite sensor was designed and fabricated to detect insect infestation. This sensor was cost efficient, easy to fabricate and was highly stable in air. When an organic vapor is present, the carbon/polymer active layer swells creating a discontinuity in the conducting pathway between adjacent carbon particles, increasing the resistance of the film. When the analyte is no longer present, the polymer will return to its original state, showing a decrease in resistance. A variety of Carbon/black polymer sensors with varying chemical characteristics could be created by using different polymer matrices. Polyethylene-co-vinyl acetate was chosen as the best polymer for this particular application based on its swelling ability in the presence of plant volatiles compared to other polymers. When the carbon concentration of the active layer was low enough to be near the percolation threshold, the sensor can be used as a “chemical switch”. The resistance of the sensor increased significantly mimicking a “switch off” response when exposed to the analyte vapor. When the analyte vapor was no longer present the sensor returned back to its original condition, showing a “switch on” response. The percolation point was obtained when the carbon concentration of the carbon/polymer composite was kept between 0.5-1 wt%. The sensor was tested and found to be sensitive to a variety of volatile organic compounds emitted during insect infestation including γ-terpinene, α-pinene, p-cymene, farnesene, and limonene and cis-hexenyl acetate.

A self-assembly driven process to synthesize island-structured dielectric films is presented. An intermetallic reaction in platinized silicon substrates provides preferential growth sites for the complex oxide dielectric (strontium-doped lead zirconate titanate) layer. Microscopy and spectroscopy analyses have been used to propose a mechanism for this structuring process. This provides a simple and scalable process to synthesize films with increased surface area for sensors, especially those materials with a complex chemistry.

The use of nanotechnology based materials for chemical sensing has been of great interest since nanocrystalline materials have been shown to offer improved sensor sensitivity, stability, and response time. Several groups are successfully integrating nanostructures such as nanowires into operational sensors. The typical procedure may include random placement (e.g., dispersion, with fine-line patterning techniques used to create functional sensors) or time consuming precise fabrication (e.g., mechanical placement using an atomic force microscope or laser tweezer techniques). Dielectrophoresis has also been utilized, however it can be challenging to achieve good electrical contact of the nanostructures to the underlying electrodes. In this paper we report on a sensor platform that incorporates nanorods in a controlled, efficient, and effective manner. Semiconducting SnO2 nanorods are used as the sensing element for detection of hydrogen (H2) and propylene (C3H6) up to 600oC. Using a novel approach of combining dielectrophoresis with standard microfabrication processing techniques, we have achieved reproducible, time-efficient fabrication of gas sensors with reliable contacts to the SnO2 nanorods used for the detection of gases. The sensor layout is designed to assist in the alignment of the nanorods by selectively enhancing the electric field strength and allowing for the quick production of sensor arrays. The SnO2 nanorods are produced using a thermal evaporation-condensation approach. After growth, nanorods are separated from the resulting material using gravimetric separation. The rods vary in length from 3μm to greater than 10μm, with diameters ranging from 50 to 300nm. Dielectrophoresis is used to align multiple nanorods between electrodes. A second layer of metal is incorporated using standard microfabrication methods immediately after alignment to bury the ends of the rods making contact with the underlying electrodes within another layer of metal. Electrical contact was verified during testing by the response to H2 and C3H6 gases at a range of temperatures. Testing was performed on a stage with temperature control and probes were used for electrical contact. Gas flows into the testing chamber at a flow rate of 4000sccm. Sensor response of normalized current shift, |Igas-Iair|/Iair, was measured at a constant voltage bias. Sensors showed response to both H2 and C3H6. Detection of H2 was achieved at 100oC and response levels improved approximately 12000-fold at 600oC. Detection of C3H6 started at 100oC and improved approximately 10000-fold at 600oC. Detection of at least 200ppm for both gases was achieved at 600oC. Using this novel microfabrication approach, semiconducting SnO2 nanorods integrated into a microsensor platform have been demonstrated and sensing response showed dramatic increases at higher temperatures.

A novel, flexible and ductile organic field-effect transistor (OFET) able to detect pH changes in chemical solutions has been realized and successfully tested. With respect to other organic pH sensors, based on an ISFET-like structure, in our approach the organic transistor is completely separated from the sensing active area and its gate is left floating. The device is biased with a fourth electrode (control-gate) capacitively coupled to the floating-gate. The floating-gate is functionalized by deposition of a layer of thio-amines able to protonize proportionally to the pH value of the solution thus modulating the drain current. The structure does not need an Ag/AgCl counter-electrode since the control-gate is not in contact with the solution. Moreover, the sensing mechanism does not depend on the choice of the dielectric and semiconductor material since the working principle is based on charge separation in the metal induced by the electric field. This structure also simplifies the realization of the fluidics since all the contactable electrodes (drain, source and control-gate) are on the same side of the substrate. A differential measurement approach was adopted in order to get rid of device aging and process-related fluctuations. With the same structure, other chemical species may be detected provided that a proper functionalization procedure is adopted.

Polymer nanocomposite gratings with a 363 nm period and a 12 nm step height were replicated using a glass master in a rapid, low-pressure imprint process. The composite materials were based on a UV-curable acrylated hyperbranched polymer and nanosized SiO2 particles. The influence of particle fraction up to 25 vol%, process pressure and UV intensity on the grating geometry was analyzed using atomic force microscopy. The period of the grating was found to be identical to that of the glass master for all investigated conditions. It was shown that the gel point of the nanocomposite was an important factor that determined the stability as well as the dimensions of the imprinted structure. However, a distortion of the grating was observed with increasing fraction of SiO2, which was correlated to the increased internal stress of the composite. Wavelength interrogated optical sensors were produced by depositing a high refractive index TiO2 layer on the composite gratings. The laser signal strength of the polymer sensors was equal to that of the reference high precision glass sensor with 10-12 g/mm2 sensitivity. The strength was lower for the nanocomposites due to propagation losses argued to result from residual porosity.

Properties such as semicondutor film grain size, morphology, and channel length are known to effect the sensing response in pentacene based organic thin film transistors (OTFTs). The sensing behavior for low and high mobility pentacene devices are reported here exhibiting different temperature dependent behaviors. The lower mobility OTFT exhibits an expected thermally activated response during alcohol testing with an increasing mobility with temperature along with a decreasing mobility at each temperature for increasing concentration. The higher mobility device exhibits a decrease in mobility with increasing temperature along with a decrease in mobility with increasing concentration at each temperature. In both sets of devices, the polar analyte produced reductions in drain current and shifts in threshold voltage.

Using different pressures of nitrogen, N-doped ZnO nanorod arrays of various densities have been synthesized on quartz substrates by pulsed laser deposition techniques. The nanorods grow preferentially perpendicular to the quartz surface. X-ray diffraction patterns revealed some degradation of the crystal structure at elevated nitrogen pressures. High concentrations of nitrogen doping in ZnO nanorods were estimated by X-ray photoelectron spectroscopy. Raman scattering spectra confirmed the wurtzite structure of N-doped ZnO nanorods. A prototype sensor based on the N-doped ZnO nanorod arrays demonstrates a linear dependence of the conductivity with operating temperature and pressure of a test gas pollutant.