Design, Optimization and Characterization of Metal Oxide Nanowire Sensors

En aquesta tesi, he estudiat i desenvolupat un mètode de deposició química en fase vapor assistit per aerosol (AACVD), per al creixement directe de nanoagulles d'òxid de tungstè funcionalitzades o intrínseques. Els dipòsits s'han realitzat sobre diferents substrats trasndcutors per a la seva aplicació a la detecció de gasos. Aquesta tècnica ofereix la possibilitat de co-dipositar els metalls amb els òxids metàl•lics emprant una sola etapa de deposició. La síntesi del material nanoestructurat, la fabricació del dispositiu, la caracterització dels materials i la detecció de gasos han estat investigades. El mètode AACVD es va emprar per al creixement i la integració directa de la pel•lícula sensible sobre substrats ceràmics (alúmina), MEMS (micro hotplates) i polimèrics flexibles, el que demostra la seva compatibilitat i idoneïtat per al creixement de nanoestructures d'òxid metàl•lics sobre una àmplia gamma de substrats transductors. A més, el mètode AACVD s'ha implementat també en un reactor de paret freda per créixer les nanoestructures de WO3, emprant l'escalfament localitzat que permeten aconseguir les microresistencias calefactores integrades en alguns dels transdcutors emprats. Totes les pel•lícules sintetitzades en aquesta tesi doctoral es componien de nanoagulles de WO3 pur o de WO3 funcionalitzat amb nanopartícules d'or (Au), platí (Pt), òxid de coure (Cu2O) o pal•ladi (Pd). Es van utilitzar diverses tecnologies d'anàlisi per caracteritzar la morfologia, l'estructura i la composició de les pel•lícules produïdes. Els resultats van mostrar que el nostre mètode és eficaç per al creixement de nanoagulles cristal•lines de WO3 decorades amb nanopartícules de metalls / òxids metàl•lics, a temperatures moderades (és a dir, 380 ° C), amb eficàcia en els seus costos i amb temps de fabricació curts, directament sobre l'element transdcutor amb vista a obtenir sensors de gasos. Els estudis de detecció de gasos han mostrat que aquest nanomaterial híbrid té una excel•lent sensibilitat i selectivitat en comparació amb mostres de WO3 pur. A més, els nanocompostos Cu2O / WO3 i Pd / WO3 han demostrat posseir una excel•lent sensibilitat i selectivitat cap als gasos H2S i H2, respectivament.En esta tesis, he estudiado y desarrollado un método de deposición química en fase vapor asistido por aerosol (AACVD), para el crecimiento directo de nanoagujas de óxido de tungsteno funcionalizadas o intrínsecas. Los depósitos se han realizado sobre distintos sustratos transdcutores para su aplicación a la detección de gases. Esta técnica ofrece la posibilidad de co-depositar los metales con los óxidos metálicos empleando una sola etapa de deposición. La síntesis del material nanoestructurado, la fabricación del dispositivo, la caracterización de los materiales y la detección de gases han sido investigadas. El método AACVD se empleó para el crecimiento y la integración directa de la película de sensible sobre sustratos cerámicos (alúmina), MEMS (micro hotplates) y poliméricos flexibles, lo que demuestra su compatibilidad e idoneidad para el crecimiento de nanoestructuras de óxido metálicos sobre una amplia gama de sustratos transductores. Además, el método AACVD se ha implementado también en un reactor de pared fría para crecer las nanoestructuras de WO3, empleando el calentamiento localizado que permiten conseguir las microresistencias calefactoras integradas en algunos de los transductores empleados. Todas las películas sintetizadas en esta tesis doctoral se componían de nanoagujas de WO3 puro o de WO3 funcionalizado con nanopartículas de oro (Au), platino (Pt), óxido de cobre (Cu2O) o paladio (Pd). Se utilizaron diversas tecnologías de análisis para caracterizar la morfología, la estructura y la composición de las películas producidas. Los resultados mostraron que nuestro método es eficaz para el crecimiento de nanoagujas cristalinas de WO3 decoradas con nanopartículas de metales / óxidos metálicos, a temperaturas moderadas (es decir, 380 ° C), con eficacia en sus costes y con tiempos de fabricación cortos, directamente sobre el elemento trasndcutor con vistas a obtener sensores de gases. Los estudios de detección de gases han mostrado que este nanomaterial híbrido tiene una excelente sensibilidad y selectividad en comparación con muestras de WO3 puro. Además, los nanocompuestos Cu2O / WO3 y Pd / WO3 han demostrado poseer una excelente sensibilidad y selectividad hacia los gases H2S y H2, respectivamente.In this thesis, I have studied and developed aerosol assisted chemical vapour deposition (AACVD) methods for the direct growth of non-functionalized and functionalized tungsten oxide nanoneedles, onto different transducer substrates, for gas sensing applications. This technique gives the possibility to co-deposit metals with metal oxides nanostructures within a single step deposition. The nanostructured material synthesis, device fabrication, material characterization and gas sensing performance have been investigated. AACVD method was employed for the direct growth and integration of the sensing film onto ceramic (alumina), MEMS (silicon micro hotplates) and flexible polymeric substrates, demonstrating its compatibility and suitability for growing metal oxide nanostructures onto a wide spectrum of sensor substrates. Furthermore, AACVD based on the localized heating of substrates employing their embedded resistive microheaters has been also performed and developed for the growth of WO3 nanostructures, using a cold wall reactor. All the synthesized films used in this doctoral thesis were composed of pure WO3 nanoneedles or WO3 nanoneedles functionalized with either gold (Au), platinum (Pt), cuprous oxide (Cu2O) or palladium (Pd) nanoparticles. Various analytical techniques were used to characterize the morphology, the structure and the composition of the produced films. The results showed that our method is effective for growing single crystalline WO3 nanoneedles decorated with metals/metal oxides nanoparticles at moderate temperatures (i.e., 380 °C), with cost effectiveness and short fabrication times, directly onto transducers in view of obtaining gas sensors. The gas sensing studies performed showed that these hybrid nanomaterials have excellent sensitivity and selectivity compared to pristine WO3 samples. Cu2O/WO3 and Pd/WO3 nanocomposites have shown excellent sensitivity and selectivity toward H2S and H2 gases respectively

Pd-Nanoparticle-Decorated Multilayered MoS₂ Sheets for Highly Sensitive Hydrogen Sensing

In this work, efficient hydrogen gas sensors based on multilayered p-type bare MoS2 and Pd-decorated MoS2 were fabricated. MoS2 was deposited onto alumina transducers using an airbrushing technique to be used as a sensing material. Aerosol-assisted chemical vapor deposition (AACVD) was used to decorate layered MoS2 with Pd nanoparticles at 250 °C. The bare and Pd-decorated MoS2 was characterized using field emission scanning electron microscopy (FESEM), high-resolution transmission electron microscopy (HR-TEM), X-ray diffraction (XRD), and Raman spectroscopy. The characterization results reveal the multilayered crystalline structure of MoS2 with successful Pd decoration. The size of the Pd nanoparticles ranges from 15 nm to 23 nm. Gas sensing studies reveal that a maximum response of 55% is achieved for Pd-decorated MoS2 operated at 150 °C to 100 ppm of H2, which is clearly below the explosive limit (4%) in air. The higher sensitivity due to Pd nanoparticle decoration was owed to a spillover effect. This study reveals that the sensitivity of the sensors is highly dependent on the amount of Pd decoration. Moreover, sensor responses increase slightly when exposed to 50% relative humidity (RH at 25 °C)

SnO 2 Sensors For a Portable Transdermal Alcohol Detector Via Finger

In this work we report, for the first time, on the fabrication of portable transdermal alcohol detector device, based on lab made tin oxide (SnO 2 ) gas sensors. This method allowed us the continuous monitoring of alcohol in a non-invasive way with low cost and easy fabrication process. From the calibration results, the fabricated sensors exhibited high sensitivity, with fast detection and good stability, toward a wide range of ethanol concentrations. Additionally, they showed high immunity to elevate relative humidity percentages. Real time transdermal alcohol monitoring was performed on a volunteer. Twenty minutes after drinking 50 ml of tequila, the skin starts to emit alcohol and the sensor resistance begins to decrease. Alongside to this, breath alcohol measurements were simultaneously collected by using DRAGGER 6820 certified breathalyzer. The results revealed a consistent correspondence between the kinetics of blood, breath and perspiration, which validate the developed device reported in this work

Embedded Transdermal Alcohol Detection via a Finger Using SnO2 Gas Sensors

International audienceIn this paper, we report the fabrication and characterization of a portable transdermal alcohol sensing device via a human finger, using tin dioxide (SnO2) chemoresistive gas sensors. Compared to conventional detectors, this non-invasive technique allowed us the continuous monitoring of alcohol with low cost and simple fabrication process. The sensing layers used in this work were fabricated by using the reactive radio frequency (RF) magnetron sputtering technique. Their structure and morphology were investigated by means of X-ray spectroscopy (XRD) and scanning electron microscopy (SEM), respectively. The results indicated that the annealing time has an important impact on the sensor sensitivity. Before performing the transdermal measurements, the sensors were exposed to a wide range of ethanol concentrations and the results displayed good responses with high sensitivity, stability, and a rapid detection time. Moreover, against high relative humidity (50% and 70%), the sensors remained resistant by showing a slight change in their gas sensing performances. A volunteer (an adult researcher from our volunteer group) drank 50 mL of tequila in order to realize the transdermal alcohol monitoring. Fifteen minutes later, the volunteer’s skin started to evacuate alcohol and the sensor resistance began to decline. Simultaneously, breath alcohol measurements were attained using a DRAGER 6820 certified breathalyzer. The results demonstrated a clear correlation between the alcohol concentration in the blood, breath, and via perspiration, which validated the embedded transdermal alcohol device reported in this wor

How the Chamber Design Can Affect Gas Sensor Responses

In this paper, we report the significant role played by the testing chamber for measuring the true gas sensor responses. Two different designs were studied and compared. The first one has a cross-shape in which the direction of gas flow is perpendicular to the sensor surface. The second one has a boat-shape in which the gas flow is tangential to the sensor surface. The results demonstrated that contrarily to the cross-shape chamber, the gas concentration is highly homogenous and equal to the set point in the boat-shape chamber. Additionally, the sensor responses are much stable, faster and higher. Besides, all the mathematical modeling and simulation results are in a good agreement with the experimental studies, which allow the validation of the proposed boat-shape chamber model

An ultrasensitive room-temperature H2S gas sensor based on 3D assembly of Cu2O decorated WS2 nanomaterials

Herein, we report for the first time on the fabrication of a hybrid material consisting of Cu2O nanoparticlesdecoratedmultilayeredtungstendisulfide nanostructuresand demonstrate their remarkable gas sensing characteristics towards hydrogen sulfide gas. In the first step, a continuous film of WS2 was deposited directly on commercial alumina substrate by adopting a facile route combining aerosol-assisted chemical vapor deposition with H2 free atmospheric pressure CVD technique. For functionalization an additional step of synthesis was added where copper oxide nanoparticles were grown and deposited directly over as-grown tungsten disulfide at low temperature (i.e., 150 ◦C) using a simple and cost-effective technique. The morphological, structural and chemical characteristicswere investigatedusing FESEM, TEM, and EDX spectroscopy.The gas-sensing studies performed shows that this hybrid nanomaterial has excellent sensitivity towards hydrogen sulfide (11-times increase in response compared to that of pristine WS2 sensor) at moderate temperature (150 ◦C). Additionally, functionalization of pristine WS2 sensor with Cu2O nanoparticles further enhances the gas sensing performance towards the targeted gas even at room temperature (13-times increase in response compared with that of pristine WS2 sensor). Moreover, results obtained from humidity cross-sensitivity of Cu2O-WS2 sensor indicates superior gas sensing response (with a negligible decrease in response) as compared to pristine WS2 sensor, when ambient humidity is increased to 50%, which is rarely found in metal oxide-based sensors. This study could add a significant research value in the gas sensor domain