Fabrication of gas sensing devices with ZnO nanostructure by the low-temperature oxidation of zinc particles

A method for low-temperature synthesis of a mixture of high-density ZnO nanoflakes and nanowires was developed to produce low-cost and high-efficiency gas sensors with ZnO nanostructures. ZnO nanoflakes and nanowires were grown on glass substrates by the RF sputter deposition of Zn particles and localized oxidation at a low temperature of 300 °C. The synthesized ZnO nanoflakes and nanowires were polycrystalline and had nanometer dimensions, as revealed by X-ray diffraction (XRD) and field emission scanning electron microscope (FESEM) measuring. A gas sensor based on the mixture of ZnO nanoflakes/nanowires responded rapidly and sensitively to ethanol. The sensing properties of the ZnO nanostructure sensor were approximately 72% for 50 ppm ethanol gas at an operating temperature of 100 °C. The response to 10 ppm of ethanol gas was 42% at the same temperature.     

Characterization of transition metal oxide ceramic material for continuous thermocouple and its use as NTC fire wire sensor

The ceramic powder prepared from the mixture of Mn₃O₄ and La₂O₃ have been characterized for NTC behavior and the same have been used as CT²C (continuous thermocouple) sensor in the form of a thin metal cable to detect over-heating. These materials have mega ohm resistance at room temperature and showed exponential drop in resistance with the rise in temperature over a temperature range of 100–400 °C. It has been observed that as the concentration of La₂O₃ increases from 0 to 10% the NTC behavior drops from (400–260 °C) ±10%. The material was pressed into pellets and sintered at 700 °C for 3 h resulting in good bonding strength. Electrical characterization of the material was done by measuring the resistance over a temperature range of 100–400 °C. The material showed reproducible NTC characteristics over the temperature range 400, 370, 340, 280, and 260 °C with decreasing thermistor constant values (B = 9588, 9210, 8500, 5170, 3330 K⁻¹) and activation energy (ΔE = 826, 794, 733, 445, 287 meV), respectively. The decrease in activation energy of the ceramic powder with increase in La₂O₃ concentration makes it possible to fabricate thermal sensors which can be used in different temperature ranges. The microstructure was studied using SEM and evidence of a sintered body with grain size around 1 μm was observed in the material. XRD analysis indicated the single-phase tetragonal structure of the ceramic material. The process of using this ceramic material for fabrication of 10 ft continuous fire wire sensor has been explained.     

Temperature compensation of fluorescence intensity-based fiber-optic oxygen sensors using modified Stern–Volmer model

In practical sensing applications, temperature effects are of particular concern, and hence it is necessary to develop the means to correct the fluorescence intensity measurement in accordance with the working temperature. Accordingly, this study develops a modified Stern–Volmer model to compensate for the temperature drift of oxygen concentration measurements obtained using fiber-optic sensors. The oxygen sensors considered in this study are based on teraethylorthosilane (TEOS)/n-octyltriethoxysilane (Octyl-triEOS) or n-propyltrimethoxysilane (n-propyl-TriMOS)/3,3,3-trifluoropropyltrimethoxysilane (TFP-TriMOS) composite xerogels doped with platinum meso-tetrakis(pentafluorophenyl)porphine (PtTFPP).

The experimental results are fitted to the modified Stern–Volmer model in order to compute suitable values for a temperature compensation coefficient at different working temperatures. It is found that the proposed temperature compensation method reduces the difference in the oxygen concentration measurement for working temperatures in the range of 25–70 °C as compared to data without compensation. The linearity and sensitivity of PtTFPP-doped n-propyl-TriMOS/TFP-TriMOS sensor are better than PtTFPP-doped TEOS/Octyl-triEOS sensor for working temperatures in the range of 25–70 °C.

The proposed approach could provide a straightforward and effective means of improving the accuracy of fiber-optic oxygen sensors if a variable attenuator is designed according to the temperature compensation coefficient. Thus, the fiber-optic oxygen sensor with a variable attenuator could work in a broad temperature range without using a temperature sensor.     

Ceria-doped SnO2 sensor highly selective to ethanol in humid air

In our earlier study, we reported that at 300 °C, a 2.0 wt.% CeO₂-doped SnO₂ sensor is highly selective to ethanol in the presence of CO and CH₄ gases [F. Pourfayaz, A. Khodadadi, Y. Mortazavi, S.S. Mohajerzadeh, CeO₂ doped SnO₂ sensor selective to ethanol in presence of CO, LPG and CH₄, Sens. Actuators B 108 (2005) 172–176]. In the present investigation, we report the influence of ambient air humidity on the ethanol selective SnO₂ sensor doped with 2.0 wt.% CeO₂. Maximum response to ethanol occurs at 300 °C which decreases with the relative humidity. The relative humidity was changed from 0 to 80% for different ambient air temperatures of 30, 40 and 50 °C and the response of the sensor was monitored in a 250–450 °C temperature range. As the relative humidity in 50 °C air increased from 0 to 30%, a 15% reduction in the maximum response to ethanol was observed. A further increase in the relative humidity no longer reduced the response significantly. The presence of humidity improved the sensor response to both CO and CH₄ up to 350 °C after which the extent of improvement became smaller and at 450 °C was almost diminished. The sensor is shown to be quite selective to ethanol in the presence of humid air containing CO and CH₄. The selectivity passes a maximum at 300 °C; however it declines at higher operating temperatures.     

Highly sensitive gas sensors based on hollow SnO2 spheres prepared by carbon sphere template method

Hollow SnO₂ spheres were prepared in dimethylfomamide (DMF) by controlled hydrolysis of SnCl₂ using newly made carbon microspheres as templates. The phase composition and morphology of the material particles were characterized by means of X-ray diffraction (XRD) and scanning electron microscopy (SEM), respectively. The gas sensing properties of sensors based on the hollow SnO₂ spheres were investigated. It was found that the sensor exhibited good performances, characterized by high response, good selectivity and very short response time to dilute (C₂H₅)₃N operating at 150 °C, especially, the response to 1 ppb (C₂H₅)₃N attained 7.1 at 150 °C. It was noteworthy that the response to 0.1 ppm C₂H₅OH of the sensor was 2.7 at 250 °C.     

Quartz rate gyro sensor for automotive control

A new quartz rate gyro sensor has been developed for automotive controls. The principle of the sensor is detection of the Coriolis force with a vibrator. An H shape vibrator supported with a stem at its center was used. The vibrator supported at the center was good for the isolation of a small detection motion from a large excitation motion. A new mechanical coupling model and the FEM analysis were used to reduce output offset of the sensor. The detection range of the sensor is from −100 to 100°/s. The sensor output offset is small within ±1°/s in the wide temperature range from −30 to 85 °C. The developed quartz rate sensor satisfied required specifications and wide temperature stability.     

TiO2 thin films from titanium butoxide: Synthesis, Pt addition, structural stability, microelectronic processing and gas-sensing properties

TiO₂ thin films were prepared by spin-coating of a Ti butoxide-derived sol onto oxidized silicon wafers, followed by a heat-treatment at temperatures ranging from 500 to 800 °C. The film thickness after heat-treatment at 500 °C was 50 nm. Pt addition, with a Pt:Ti nominal atomic ratio ranging from 0.01 to 0.1, was achieved by adding solutions of Pt(II) acetylacetonate to the TiO₂ sols. The thin films were investigated by X-ray diffraction, evidencing that Pt promoted the structural transformation of the starting anatase phase of TiO₂ to rutile, with a more enhanced effect with increasing the Pt concentration and/or the heat-treatment temperature. High-resolution transmission electron microscopy evidenced that, when a Pt:Ti atomic ratio of 0.05 and a heat treatment at 500 °C were used, the TiO₂ contained both anatase and rutile phases and interspersed Pt nanocrystals (2–3 nm). This result allowed attributing the structural transformation in TiO₂ to the strain created by the Pt nanocrystals—a conclusion which was further corroborated by the observation that Pd-modified films, prepared under similar conditions, were only composed of anatase TiO₂ and did not contain any Pd nanocrystals. The films heat-treated at 500 °C were able to withstand a full microelectronic processing sequence, including dry etching for gas sensors sensitive area definition, Ti/Pt contact formation, and heater processing on the backside of the sensor substrates. H₂ gas-sensing tests evidenced that the anatase TiO₂ phase was much more sensitive than the rutile one. The presence of Pt further enhanced the gas-sensing properties, lowering the optimum sensor operation temperature to about 330 °C and allowing for the detection of a minimum H₂ concentration of about 1000 ppm.     

Characterization of miniaturized one-side-electrode-type fluid-based inclinometer

In this study, electrical double-layer theory is applied to realize a one-side-electrode-type fluid-based inclinometer combined with complementary metal oxide semiconductor (CMOS) circuitry. Substrate penetration lithography was applied in the fabrication of high-aspect-ratio SU-8 container molds, and molds with heights 1.0 mm were fabricated. Polydimethylsiloxane (PDMS) was used as the container material, and electrodes were fabricated on a ceramic substrate. Considering the electrical double-layer property, low surface tension, the dielectric constant and the problem of volatilization, methanol and propylene carbonate were tested as electrolytes. A charge-balanced capacitance–voltage (C–V) conversion circuit was designed as a detection circuit for this sensor and it was fabricated using 0.35 μm CMOS technology. The sensor part and detection circuit were integrated in one ceramic packaging for realize a miniaturization of inclination sensor system. To overcome the surface tension of the PDMS surface, silicone oil was injected in the container to cover the entire inner surface so that the movement of solution in the container became smooth. The linearity of the analog output of ±60° inclination for container dimensions of Ø 4.0 mm × 1.0 mm (diameter × thickness) was less than 6%/F.S. The minimum moving angle and response time were 0.4° and 0.9 s, respectively, when propylene carbonate was used as the electrolyte. The change in temperature did not affect the output voltage of the sensor between 0 and 50 °C. The effect of vibration was demonstrated in this paper.     

Microstructure, electrical and ethanol-sensing properties of perovskite-type SmFe0.7Co0.3O3

Ultrafine SmFe_0.7Co_0.3O₃ powder, prepared by a sol–gel method, shows a single-phase orthogonal perovskite structure. The influence of annealing temperature upon its crystal cell volume, microstructure, electrical and ethanol-sensing properties was investigated in detail. When the annealing temperature increases from 600 to 950 °C, the unit cell volume of the SmFe_0.7Co_0.3O₃ sample reduces, and its average grain size increases. When the annealing temperature increases from 600 to 850 °C, the optimal working temperature and response to ethanol of the SmFe_0.7Co_0.3O₃ sensor increase, and the response–recovery time shortens. But when the annealing temperature further increases from 850 to 950 °C, there are decreases of the optimal working temperature and sensor response, and the response–recovery time is prolonged. The results indicate that, as for sensor response, its optimal annealing temperature is about 850 °C, and the sensor based on SmFe_0.7Co_0.3O₃ annealed at 850 °C shows the highest response S = 80.8 to 300 ppm ethanol gas, and it has the best response–recovery and selectivity characteristics. When the ethanol concentration is as low as 500 ppm, the curve of its optimal response versus concentration is nearly linear. Meanwhile, the influence mechanisms of annealing temperature upon the conductance, the optimal working temperature and sensor response for SmFe_0.7Co_0.3O₃ were studied.     

Room temperature synthesis of γ-Fe2O3 by sonochemical route and its response towards butane

Nanocrystalline gamma iron oxide (γ-Fe₂O₃) has been synthesized at room temperature through sonication-assisted precipitation technique. The key in obtaining γ-Fe₂O₃ at room temperature lies in exploiting high-power ultrasound (600 W). The gas-sensing properties to n-butane of pure γ-Fe₂O₃ were investigated by studying the electrical properties of the sensor elements fabricated from the synthesized powder. The maximum response (90%) of the sensor to 1000 ppm n-butane at 300 °C can be explained on the basis of catalytic activity of the nanocrystallites. The response and recovery time of the sensor to 1000 ppm n-butane were less than 12 s and 120 s, respectively.     

Highly sensitive and fast responding CO sensor using SnO2 nanosheets

A highly sensitive and fast responding CO sensor was fabricated from a sheet-like SnO₂. The SnO sheets were prepared by a room temperature reaction between SnCl₂, hydrazine and NaOH, and they were subsequently oxidized into SnO₂ sheets at high temperature (600 °C). The morphology and size of the SnO₂ sheets could be controlled during the formation of SnO, which influence the sensor response (R_a/R_g) and response time to a great extent. The sensor response of SnO nanosheets to 10 ppm CO was enhanced up to 2.34, and the 90% sensor response time could be reduced to 6 s, which are significantly higher and shorter than those of SnO₂ powders (1.57 and 88 s), respectively. The realization of both a high sensitivity and rapid response were explained in terms of rapid gas diffusion onto the entire sensing surface due to the less-agglomerated and very thin structure of SnO₂ nanosheets and the catalytic effect of Pt.     

A novel thick-film ceramic humidity sensor

The paper describes the results of studies on the fabrication and characterisation of a thick-film humidity sensor based on the semiconducting metal oxide MnWO₄. The sensor element possesses a novel ‘sandwich’-configuration with a 40 μm porous MnWO₄ ceramic layer sandwiched by two 10 μm polarity-reversed, interdigitated metal films. Instead of traditional glass frits, LiCl powders are used as adhesion promoters for sintering the sensor paste. With this method, MnWO₄ powders with an average particle size of 3.0 μm are sintered at the standard thick-film firing temperature of 850°C. The sintered ceramic layer exhibits a porous structure. The novel electrode arrangement combines the advantages of humidity sensors in the form of a parallel capacitor with those in the form of an interdigital capacitor, permitting a high sensitivity and a fast response. The influence of temperature on the sensor characteristics has been compensated for by integrating a thick-film NTC resistor. The humidity sensor shows no cross-sensitivity to organic vapour. The organic contamination on the sensor surface can be burned out by heating the sensor element at about 400°C with the refresh heater printed on the back side of the substrate.     

Humidity sensing and electrical properties of a composite material of nano-sized SiO2 and poly(2-acrylamido-2-methylpropane sulfonate)

A composite material of nano-sized SiO₂ and poly(2-acrylamido-2-methylpropane sulfonate) (poly(AMPS)) was used to make a humidity sensor. The infrared (IR) spectra and microstructure of the material were analyzed, and the humidity sensing and electrical properties of the sensor were measured. The sensor well responded to humidity with a relative good linearity, though it depended on the applied frequency. The temperature influence between 15 and 35 °C was −0.71 and −0.15% RH/°C at 30 and 90% RH, respectively. The sensor showed a negligible hysteresis and fast response time upon humidification and desiccation. The stability of the sensor in a highly humid and alcoholic environment increased with increasing the SiO₂ content. The activation energy for conduction reduced with water adsorption. The different impedance plots observed at low and high relative humidity suggested different sensing mechanisms of the SiO₂/poly(AMPS) composite material.     

Cerium oxide/SnO2-based semiconductor gas sensors with improved sensitivity to CO

SnO₂-based semiconductor gas sensors have been successfully fabricated and tested for detecting carbon monoxide and methane. The sensitivity and selectivity of the sensors are tailored by incorporation of different additives such as platinum and cerium oxide. While platinum enhances the sensor response to CH₄, ceria suppresses its sensitivity in favor of carbon monoxide. The effect of operating temperature on the performance of sensors is reported. Addition of 10% cerium oxide in the SnO₂ sample leads to an insignificant response to methane even at an elevated temperature of 450°C, while its response to CO remains intact.     

Potentiometric CO2 gas sensor with lithium phosphorous oxynitride electrolyte

Potentiometric cell, Au/LiCoO₂ 5 m/o Co₃O₄/Li_2.88PO_3.73N_0.14/Li₂CO₃/Au, has been fabricated and investigated for monitoring CO₂ gas. A LiCoO₂–Co₃O₄ mixture was used as the solid-state reference electrode instead of a reference gas. The idea is to keep the lithium activity constant on the reference side using thermodynamic equilibrium at a given temperature. The thermodynamic stability of the reference electrode was studied from the phase stability diagram of Li–Co–C–O system. The Gibb’s free energy of formation of LiCoO₂ was estimated at 500°C from the measured value of the cell emf. The sensors showed good reversibility and fast response toward changing CO₂ concentrations from 200 to 3000 ppm. The emf values were found to follow a logarithmic Nernstian behavior in the 400–500°C temperature range. CH₄ gas did not show any interference effect. Humidity and CO gas decreased the emf values of the sensor slightly. NO and NO₂ gases affect this sensor significantly at low temperatures. However, increased operating temperature seems to reduce the interference.     

The intelligent knee sleeve: A wearable biofeedback device

A unique textile-based device, the intelligent knee sleeve (IKS), uses conducting polymer technology to provide feedback on knee flexion angle for injury prevention programs. After identifying the most appropriate base fabric for the sensor, 12 athletes (age = 26.1 ± 3.2 years) performed four landing movements while wearing the sleeve, which was set to provide audible feedback at 25° and 45° knee flexion. Sensor and audible output (1000 Hz), knee kinematics (200 Hz) and ground reaction forces (1000 Hz) were recorded during the landing movements using an OPTOTRAK^® motion analysis system. Paired t-tests and intraclass correlation coefficients were used to determine validity and reliability of the feedback. The results revealed that the audible feedback tone was able to significantly differentiate between different goniometer-programmed knee angles (25° and 45°). Knee angles computed using the kinematic data from each trial for each movement were also highly reliable (intraclass correlation coefficients, R₁ = 0.903–0.988). It was concluded that although the IKS provides valid and reliable feedback on knee flexion angle, consistent feedback is dependent upon use of a sensor unaffected by environmental conditions. Such wearable biofeedback systems have application in a broad spectrum of activities, including performance enhancement, injury prevention and rehabilitation.     

Selective detection of ethanol vapor and hydrogen using Cd-doped SnO2-based sensors

The effect of CdO doping on microstructure, conductance and gas-sensing properties of SnO₂-based sensors has been presented in this study. Precursor powders with Cd/Sn molar ratios ranging from 0 to 0.5 were prepared by chemical coprecipitation. X-ray diffraction (XRD) analysis indicates that the solid-state reaction in the CdO–SnO₂ system occurs and -CdSnO₃ with pervoskite structure is formed between 600 and 650°C. CdO doping suppresses SnO₂ crystallite growth effectively which has been confirmed by means of XRD, transmission electron microscopy (TEM) and BET method. The 10 mol% Cd-doped SnO₂-based sensor shows an excellent ethanol-sensing performance, such as high sensitivity (275 for 100 ppm C₂H₅OH), rapid response rate (12 s for 90% response time) and high selectivity over CO, H₂ and i-C₄H₁₀. On the other hand, this sensor has good H₂-sensing properties in the absence of ethanol vapor. The sensor operates at 300°C, the sensitivity to 1000 ppm H₂ is up to 98, but only 16 and 7 for 1000 ppm CO and i-C₄H₁₀, respectively.     

A low-cost inductive proximity sensor for industrial applications

In this paper, we present an inductive proximity sensor with fully integrated electronics. The sensor with the compact hybrid configuration is composed of a sensing flat coil and an integrated electronic interface. We focused during the development on the temperature stability and robustness of the sensor by keeping its low-fabrication cost. The sensor exhibits a longitudinal resolution of 120 nm for an aluminum target position up to 500 μm from the sensing coil with the side size of 3.5 mm. The temperature drift of the sensor is less than 700 ppm/°C for the same range of the target position. The total working range is from 100 to 1500 μm. The sensor power consumption is 100 mW and the active sensor dimensions are 3.5 mm×3.5 mm×1.2 mm. We also showed the facility of the sensor packaging. This kind of integrated sensor has the potential for even more industrial applications.     

Sol–gel derived polycrystalline Cr1.8Ti0.2O3 thick films for alcohols sensing application

The powder sample of Cr_1.8Ti_0.2O₃ (CTO) was obtained by a sol–gel method. The thick films were developed on identical ceramic tubes of 4 mm length comprising of two Au-electrodes and printing an eight-layer film prepared by mixing CTO with glass powder and -terpinol as an organic vehicle. X-ray powder diffraction (XRD) patterns showed the formation of a single phase. The scanning electron microscope (SEM) images of the ceramic sensor treated at 850 °C revealed that the grain size was larger than 400 nm for the individual isolated grains on the surface, and the agglomerated dense spheroidal platelets had the size of 1–4 μm in diameter. The AC impedance measurement in ambient air showed that the resistance decreased nearly by two orders of magnitude with an increase in temperature in the range of 400–600 °C for both the powder sample and the thick film, and the activation energy E_a derived from the measurement was found to be 0.35 and 0.36 eV for the powder and the film, respectively. The films were exposed to various concentrations of alcohols (0.4–1.2 ppm of methanol and 1.0–5.0 ppm of ethanol), followed by determination of sensor response, sensitivity and reversibility and reproducibility. The origin of the gas response was attributed to the surface reaction of R-OH (R = methyl and ethyl group) with O⁻_(ads) to form adsorbed R-CHO, which was desorbed as a gas at 400 °C after the sensor departing from the gas.     

Influence of Pd doping on morphology and LPG response of SnO2

In the present study nanocrystalline pristine and Pd-doped SnO₂ (Pd:SnO₂) with various mol% Pd have been synthesized by a modified Pechini citrate route. Transmission electron microscopy and X-ray powder diffraction studies were used to characterize the morphology, crystallinity, and structure of the SnO₂ and Pd:SnO₂. The response of the pristine SnO₂ and Pd:SnO₂ was studied towards different reducing gases. The 1.5 mol% Pd doping showed an enhanced response of 75 and 95% towards LPG at as low as 50 and 100 °C, respectively, which were quite large high value as compared with pristine SnO₂ (38 and 35% at 50 and 100 °C, respectively). Structural characterization revealed that Pd doping reduced the crystallite size of SnO₂ and helps in the formation of distinct spherical nanospheres at a calcinations temperature of 500 °C. Thus the increase in LPG response can be correlated with the spherical morphology, a decrease in the crystallite size (11 nm) due to doping with Pd as compared with the pristine SnO₂ (26 nm) and main role of Pd as a catalyst.