This research was born from NASA Kennedy Space Center’s (KSC) need for passive, wireless and individually distinguishable cryogenic liquid and H2 gas sensors in various facilities. The risks of catastrophic accidents, associated with the storage and use of cryogenic fluids may be minimized by constant monitoring. Accidents involving the release of H2 gas or LH2 were responsible for 81% of total accidents in the aerospace industry. These problems may be mitigated by the implementation of a passive (or low-power), wireless, gas detection system, which continuously monitors multiple nodes and reports temperature and H2 gas presence. Passive, wireless, cryogenic liquid level and hydrogen (H2) gas sensors were developed on a platform technology called Orthogonal Frequency Coded (OFC) surface acoustic wave (SAW) radio frequency identification (RFID) tag sensors. The OFC-SAW was shown to be mechanically resistant to failure due to thermal shock from repeated cycles between room to liquid nitrogen temperature. This suggests that these tags are ideal for integration into cryogenic Dewar environments for the purposes of cryogenic liquid level detection. Three OFC-SAW H2 gas sensors were simultaneously wirelessly interrogated while being exposed to various flow rates of H2 gas. Rapid H2 detection was achieved for flow rates as low as 1ccm of a 2% H2, 98% N2 mixture. A novel method and theory to extract the electrical and mechanical properties of a semiconducting and high conductivity thin-film using SAW amplitude and velocity dispersion measurements were also developed. The SAW device was shown to be a useful tool in analysis and characterization of ultrathin and thin films and physical phenomena such as gas adsorption and desorption mechanisms.

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I dagsläget finns det ingen standardiserad metod för att mäta en enhets tillstånd medhjälp av dofter. Vid tillståndsövervakning av rullningslager är vibrationsmätning denmest dominanta metoden. I samband med vibrationsmätning används i vissa falltemperaturövervakning för att få en bättre insikt på rullningslagrets tillstånd. I det härarbetet undersöks de om en elektronisk näsa kan avgöra ett rullningslagers tillstånd.Innan några mätningar påbörjas monterades en elektronisk näsa ihop i ett hölje sombestår av ett kretskort, metalloxid-sensorer och en fläkt för att styra dofter med ettkonstant flöde mot sensorerna. Den elektroniska näsan styrs av en Arduino Nanomikrokontroller. Utöver e-näsan sättes en enhet ihop tillhörande två temperaturgivareoch en luftfuktighetsgivare som styrs av en Arduino UNO. Enhetens syfte är att kunnakontrollera de rådande förhållandena vid mätningar och för att leta någon form avkorrelation mot e-näsan vid eventuella utslag. Förstörande prover av kullager utfördesför att se om e-näsan reagerar innan ett lagerhaveri. Testerna gjordes i en öppen samtsluten miljö och tre stycken olika oljor används för att smörja lagret. Detta för att seom e-näsan reagerar olika beroende på vilken olja som används. En undersökningutförs ifall den elektroniska näsan kan separera på de tre oljorna som används ilagertesterna. För att utvärdera mätresultaten används Excel och Minitab, därprincipalkomponentanalyser genomförs på all mätdata. Efter att alla lagerprover harverkställts utfördes en uppföljning av rullningslagrena för att studera deras tillstånd,detta genom ett optiskt mikroskop.Det framgår i rapporten att med hjälp av analysmetoden PCA syns det att denelektroniska näsan kunde skilja på hydraulolja, motorolja och växellådsolja. Utslag iPCA för de olika mätserierna blev inte identiska men det blev tydligaklusterindelningar hos samtliga mätserier. Genomförd studie visade att med delagerhaveri samt temperaturer går det inte att avgöra ett kullagers tillstånd med hjälpav en elektronisk näsa. Eftersom att de specifika gas-sensorerna som användes till enäsaninte gav någon form av utslag vid mätningarna. Den elektroniska näsanreagerade däremot vid totalhaveri av kullager, vilket är för sent i ett förebyggandeunderhållsperspektiv. Detta medförde att den elektroniska näsan inte kan användas förtillståndsövervakning av det specifika kullagret som användes vid denna studie. / At present, there is no standardized method of measuring a device's condition with thehelp of odors. In condition monitoring of rolling bearings, vibration measurement isthe most dominant method. In case of vibration measurement, temperature monitoringis used in some cases to get a better insight into the condition of the bearing. In thiswork, it is investigated whether an electronic nose can determine the condition of arolling bearing.Before any measurements began, an electronic nose is assembled in a housingconsisting of a circuit board, metal oxide sensors and a fan for stearing odors with aconstant flow towards the sensors. The electronic nose is controlled by an ArduinoNano which is a microcontroller. In addition to the e-nose, a unit is connected to twotemperature sensors and a humidity sensor controlled by an Arduino UNO. The unit'spurpose is to monitor the status and to look for any kind of correlation with the e-nosein case of any possible findings. Destructive specimens of ball bearings are performedto see if the e-nose responds prior to a bearing failure. Tests are conducted in an openand closed environment and three different oils are used to lubricate the bearings.This to see if the e-nose acts differently depending on the oil that is used. Aninvestigation is conducted if the electronic nose can separate the three different typesof oils that is used in the destructive bearing tests. To evaluate the measurementresults, Excel and Minitab are used, where principal component analysis is performedon all measurement data. After all bearing tests have been performed, a follow-up ofthe rolling bearings condition is performed, this through an optical microscope.The report shows that using the PCA analysis method, it appears that the electronicnose could distinguish between hydraulic oil, engine oil and gear oil. In the PCA forthe different measurement series the results did not become identical, but clusterdivisions became clear in all measurement series. Completed study showed that withthese bearing failures and temperatures, it is not possible to determine the condition ofthis ball bearer using an electronic nose. Because the specific gas sensors used for thee-nose did not give any kind of impact during the measurements. On the other hand,the electronic nose responded to a total failure of a ball bearing, which is too late in apreventative maintenance perspective. Therefore, the electronic nose cannot be usedfor condition monitoring of the specific ball bearing used in this study.

L'équipe micro-capteurs de l'IM2NP développe des capteursde gaz dont le principe de détection est basé sur la mesure de la variationde la conductance en présence de gaz. Le matériau utilisé comme élémentsensible est l'oxyde de tungstène (WO3) en couches minces. L'objet de cettethèse est donc d'étudier la surface de WO3 dans sa reconstruction c(2x2),obtenue par clivage selon la direction [001]. Cette étude a été également suivied'une étude des lacunes par des calculs ab initio basés sur la DFT, dans lesdeux approximations LDA et GGA. Ensuite, l'dsorption de molécules de gazsimples (O3, COx, NOx) sur des surfaces plus ou moins riches en oxygènea été effectuée. Pour simuler ces systèmes, nous avons fait le choix du codeSIESTA basé sur la DFT et qui présente l'avantage de pouvoir travailler. / The team of micro sensors at IM2NP mainly focuses onthe development of gas sensors based on measurement in conductancevariation in presence of gas. The material used as sensitive element istungsten oxide (WO3) thin film. The objective of present thesis is to studythe surface properties of WO3 in its reconstruction c(2x2), obtained bycleavage along the [001] direction. This study is also followed by a gapanalysis using ab initio calculations based on DFT in both LDA andGGA approximations. Then, the adsorption of molecules of simple gases((O3, COx NOx) for these surfaces (more or less rich in oxygen), is performed.To simulate these systems, we have chosen the SIESTA code based onDFT which is used for the larger number of atoms as compared to other codes.

Dentre os materiais de estrutura perovskita, o titanato de estrôncio, SrTiO3, é um dos mais conhecidos e estudado por apresentar interessantes propriedades como a ferroeletricidade, fotoluminescência, entre outras. Além disso, tem sido reportado na literatura que a adição de diferentes dopantes ao composto SrTiO3 modifica suas propriedades dando origem, por exemplo, a materiais para serem aplicados como sensores de gás ou na fotocatálise. Diferentes trabalhos encontrados na literatura descrevem a síntese do composto SrTiO3 e suas soluções sólidas através do método hidrotermal. Entretanto, poucos trabalhos tiveram como foco o estudo do precursor de Ti e do íon dopante nas propriedades estruturais, morfológicas, ópticas e elétricas destes materiais. Desta forma, este trabalho de tese teve como objetivo o estudo da influência da composição e de alguns parâmetros de síntese sobre as propriedades estruturais, morfológicas e ópticas do composto SrTiO3 preparado através do método hidrotermal assistido por microondas HAM. Inicialmente, foi realizada a síntese do composto SrTiO3 a 140oC por 10 minutos, onde se verificou a possibilidade de controlar a morfologia e a propriedade fotoluminescente das amostras através do tipo de precursor de Ti utilizado. Em uma segunda etapa do trabalho, o composto SrTiO3 foi sintetizado por tempos variando de 10 a 640 minutos. A caracterização destas amostras mostrou a formação da fase cúbica do SrTiO3 exibindo morfologia na forma de cubos, formados pelo processo de auto-organização, que tornam-se mais bem definidos com o aumento do tempo de síntese. Medidas de espectroscopia XANES e EXAFS na borda K do Ti mostraram que as amostras de SrTiO3 sintetizadas pelo método HAM apresentam um alto grau de desordem na estrutura local, caracterizada pela coexistência de unidades do tipo TiO5 e TiO6. Além disso, observou-se que o aumento do tempo de síntese leva a uma redução da intensidade fotoluminescente que foi atribuído à redução na concentração de vacâncias de oxigênio. Medidas de DRX das amostras do sistema SrTi1-xFexO3, ao nosso conhecimento pela primeira vez sintetizadas com sucesso através do método HAM, mostraram a formação da fase cúbica quando x &#8804 0,4. Medidas do espectro XANES e EXAFS revelaram a substituição Ti por íons Fe+2 e Fe+3, levando a formação de vacâncias de oxigênio as quais contribuem para a diminuição da energia do band-gap das amostras de 3,2 para 2,8 eV, bem como na total supressão da intensidade fotoluminescente das amostras. A análise por microscopia eletrônica de varredura FE-MEV mostrou a existência de partículas na forma de cubos cuja cinética de formação é influenciada pela variação da quantidade de ferro. Imagens de microscopia eletrônica de transmissão (MET) confirmaram a natureza mesocristalina destas partículas cujo mecanismo de crescimento ocorre por coalescência orientada, originada pelo processo de auto-organização. As amostras do sistema SrTi1-xFexO3 na forma de filmes finos foram avaliadas como sensores O3, NO2, NH3 e CO. As análises indicaram que os filmes depositados pela técnica de evaporação de feixe de elétrons apresentam um grande potencial para serem aplicados como sensor de gás ozônio, exibindo uma boa sensibilidade e seletividade comparada a outros tipos de materiais sensores. / Strontium titanate, SrTiO3, it is one of the most known and intensively studied perovskite compounds due its interesting properties such as ferroelectricity, photoluminescence, etc. According to the literature, the dopant addition into SrTiO3 network can create materials with desirable functions, for example, gas sensing and photocatalytic activity. Despite some authors reported the synthesis of pure or doped SrTiO3 by hydrothermal method, few studies have been devoted to investigate the effects of the Ti precursor and type of dopant ion on the structural, morphological and electrical properties of SrTiO3 compound. In this work, we investigated the influence of synthesis parameters and concentration iron on the structural, morphological and optical properties of SrTiO3 prepared by microwave-assisted hydrothermal method (MAH). Firstly, it was observed that the appropriate choice of the Ti precursor allowed the control of morphological and photoluminescence properties of SrTiO3 compound synthesized at 140oC for 10 minutes by MAH method. Next, SrTiO3 was synthesized during different treatment times varying from 10 to 640 minutes. X-ray diffraction (XRD) measurements indicate a SrTiO3 cubic perovskite structure and FE-SEM images revealed that the samples exhibit a cube-like shape formed by an assembly process, becoming well defined as a function of MAH treatment time. Ti-K edge XANES and EXAFS measurements indicated a large local structural distortion, revealed by the presence of TiO6 and TiO5 units. Moreover, we observed a reduction of the photoluminescence intensity as a function of treatment time probably due to decreasing of the oxygen vacancy concentration. To the best of our knowledge, this is the first time that the SrTi1-xFexO3 solid solution was synthesized by MAH method. XRD analyses indicated a cubic perovskite structure when x &#8804 0.4. XANES and EXAFS measurements revealed that iron ions present a mixed Fe+2/Fe+3 oxidation state and occupy preferentially the Ti4+-site. A UV-visible spectrum shows that the addition of iron reduces the value of optical gap of the 3.2 eV to 2.8 eV and consequently suppresses the photoluminescence intensity. An analysis of FE-SEM and HRTEM images point out that, independently of iron content, the nanoparticles have a cube-like morphology and are formed by a self-assembly of small primary nanocrystals. In addition, SrTi1-xFexO3 thin films were investigated as gas sensor towards O3, NO2, NH3 and CO gases The results indicate that the films deposited by electron beam deposition method exhibits a good response as ozone sensor compared to others gas sensors materials.

The objective of this research is to apply micromachined silicon-based resonant gravimetric sensors to the detection of gas-phase volatile organic compounds (VOCs). This is done in two primary tasks: 1) the optimization and application of silicon disk resonators to the detection of gas-phase VOCs, and 2) the development and application of a novel gravimetric-capacitive multisensor platform for the detection of gas-phase VOCs. In the rst task, the design and fabrication of a silicon-based disk resonator structure utilizing an in-plane resonance mode is undertaken. The resonance characteristics of the disk resonator are characterized and optimized. The optimized characteristics include the resonator Q-factor as a function of geometric parameters, and the dynamic displacement of the in-plane resonance mode. The Q-factors of the disk resonators range from 2600 to 4360 at atmosphere for disk silicon thicknesses from 7 µm to 18 µm, respectively. The resonance frequency of the in-plane resonance mode ranges from 260 kHz up to 750 kHz. The disk resonators are applied to the sensing of gas-phase VOCs using (poly)isobutylene as a sensitive layer. Limits of detection for benzene, toluene and m-xylene vapors of 5.3 ppm, 1.2 ppm, and 0.6 ppm are respectively obtained. Finally, models for the limits of detection and chemical sensitivity of the resonator structures are developed for the case of the polymer layers used. In the second task, a silicon-based resonator is combined with a capacitive structure to produce a multisensor structure for the sensing of gas-phase VOCs. Fabrication of the multisensor structure is undertaken, and the sensor is theoretically modeled. The baseline capacitance of the capacitor component of the multisensor is estimated to be 170 fF. Finally, initial VOC detection results for the capacitive aspect of the sensor are obtained.

High quality ammonium oxofluorotitanate discoid crystal is successfully grown on glass with an aqueous solution of ammonium hexafluorotitanate and boric acid at the molar ratio of 0.6. The concentration of hydrofluoric acid is less on the glass substrate surface and enhances the ammonium oxofluorotitanate nucleation growth. The growth rate is much higher than that grown on dioctadecyldimethylammonium. From the examinations of X-ray diffraction and high-resolution transmission electron microscopy, the crystal shows high crystalline quality and uniformity. Each titanium oxide octahedral is linked with fluorine and nitrogen atoms. Therefore, ammonium oxofluorotitanate has high potential to be thermally decomposed into high crystalline fluorine and nitrogen co-doped titanium oxide. A simple process for the preparation of nanocrystalline anatase phase titanium oxide converted from ammonium oxofluorotitanate by thermal treatment was developed. The nanocrystalline anatase phase titanium oxide shows a large bandgap reduction due to the co-doping of high concentrations of fluorine and nitrogen. Due to the excellent nanocrystalline quality and the co-doping of higher concentrations of fluorine and nitrogen at the thermal treatment temperature of 800 OC, it is 1.3 times the photocatalytic activities of P-25 due to the visble region usage of Hg lamp light source. The 11.2 times the visible photocatalytic activities of P-25 using blue light-emitting diode as the light source is obtained from thermal treatment temperature of 600 OC. There is one to one correspondence between carrier lifetime and photocatalytic activity. As a result, a highly reactive and visible-light-driven photocatalysis is achieved. The heterostructure of zinc selenide/titanium oxide and zinc sulfide/titanium oxide were prepared by metal-organic chemical vapor deposition on the above-prepared titanium oxide. The energy bandgap of zinc sulfide is much larger than that of titanium oxide and can act as a window for titanium oxide. It would not hinder titanium oxide absorption and preserve the role of fluorine and nitrogen co-doping. The energy bandgap of zinc selenide is near the maximum intensity of solar spectrum and acts as a sensitizer of titanium oxide. The lifetime of electron and hole pairs of heterostructure are about 240 and 207 nsec, which are longer than 65 nsec of titanium oxide prepared at 800 oC thermal treatment. Their photocatalytic activities are further improved to 2.0 and 1.5 times higher than that of commercial P-25. The photocatalysis of titanium oxide is very sensitive to the surface states. Titanium oxide surface defects can act as trapping sites for photo-induced holes and facilitate the separation of photo-induced carriers. Zinc selenide and zinc sulfide can passivate the surface well. It may say that titanium oxide surface defects removal has a negative impact. The density, height, diameter, PL wavelength and intensity of zinc selenide self-assembled quantum dots grown on zinc sulfide/gallium arsenide with the zinc sulfide thickness from 15 to 160 nm are studied. For a fixed 30 sec zinc selenide self-assembled quantum dots growth, it cannot be formed with the zinc sulfide thickness below 15 nm due to the close lattice match between zinc sulfide and gallium arsenide. The zinc sulfide/gallium arsenide is fully lattice relaxed with the zinc sulfide thickness higher than 130 nm examined by X-ray diffraction. The higher quality and density of zinc selenide self-assembled quantum dots can be obtained on zinc sulfide/gallium arsenide with the zinc sulfide thickness far beyond its critical thickness. The maximum zinc selenide self-assembled quantum dots density of 4.9 x 109 cm-2 with the strongest photoluminescence intensity is obtained at the zinc sulfide/gallium arsenide thickness of 130 nm. Clusters are formed on the surface of zinc selenide/gallium arsenide. The selenium segregation is the main mechanism for the formation of clusters. The dislocations will enhance the selenium segregation. Higher zinc selenide cluster corresponds to higher density of dislocations. The non-spherical cluster is formed from the mergence of the two clusters. High quality zinc oxide rods and zinc hydroxide slices are successfully grown on gallium arsenide with the aqueous solution of zinc nitrate and hexamethylenetetramine. The growth can be controlled by the appropriate nitric acid concentration incorporation in the solution. After thermal annealing, the zinc oxide slices transformed from zinc hydroxide slices can contribute much higher photocatalytic activity to 1.2 times to P-25.

Current gas sensor technology, although meeting the minimum requirements in many instances, suffers for a number of limitations. Hence, there is currently a considerable volume of research being undertaken at many laboratories of different countries. In the past, all chemical sensors and catalyst were optimized empirically by a trial and error method. Today, however, systematic research and development is becoming increasingly important in order to improve sensors and to find new sensing principles. Obtaining a long term stable gas sensor with improved sensitivity, selectivity, and low cost for mass production passes through fundamental research and material characterization to build new chemically sensitive devices or to improve existing ones. The bottom line in the design and manufacture of modern gas sensors is the transfer from ceramic(of Figaro type) to thin film gas sensors(TFGs). This transfer provides new opportunities for further microminiaturization, power consumption and cost reduction of gas sensors. Therefore, at the present time, thin film gas sensors are the basis for the design of the modern gas sensitive multi-parameter microsensor systems. Applications of these systems include environment, security, home systems, smart buildings, transportation, discrete manufacturing, process industries and so on. Microelectromechanical systems(MEMS) based integrated gas sensors present several advantages for these applications such as ease of array fabrication, small size, and unique thermal manipulation capabilities. MEMS based gas sensors; which are usually produced using a standard CMOS(Complimentary Metal Oxide Semiconductor) process, have the additional advantages of being readily realized by commercial foundries and amenable to the inclusion of on-chip electronics. In order to speed up the design and optimization of such integrated sensors, microheater designs for gas sensor applications have been presented as first part of the present thesis. As heater design is the key part for a gas sensor operation. So 3D simulations have been used to optimize micro-heater geometry. The application of MEMS Design Tool(COVENTORWARE) has been presented to the design and analysis of micro-hotplate (MHP) structures. Coupled Electro-thermal analysis provided an estimation of thermal losses and temperature distribution on the hotplate for realistic geometrical and material parameters pertinent to fabrication technology. Five microheater designs have been proposed in terms of different sizes and shapes in order to optimize the microhotplate structure to be used for gas sensor operation for the specified range of temperature and power consumption. To produce a gas sensor, which is able to detect LPG leak, thin films of tin oxide have been developed. FR sputtering has been used to deposit gas sensitive tin oxide thin filmls under various deposition conditions. Four different values of pressure in the range from high pressure(5 X 10-2 mbar) to lower pressure (2 X 10-3 mbar), three RF power values 50, 75, 100 W and varied oxygen percentage in sputtering atmosphere (0-18%) have been used to optimize the material properties of tin oxide thin films to study the sensitivity towards LPG. All the samples have been analyzed using various macro and microscopic characterization techniques. Extensive studies have been done on the sensor response for the samples deposited under different conditions. Finally the sample film deposited at 5 x 10-3 mbar, with applied power of 75 W in the presence of 8% oxygen, showed maximum sensitivity towards LPG.

Today there is a great deal of interest in the development of gas sensors for applications like air pollution monitoring, indoor environment control, detection of harmful gases in mines etc. Based on different sensing principles, a large variety of sensors such as semiconductor gas sensors, thermoelectric gas sensors, optical sensors and thermal conductivity sensors have been developed. The present thesis reports a detailed account of a novel method followed for the design and development of a thermoelectric gas sensor for sensing of Volatile Organic Compounds. Thermoelectric effect is one of the highly reliable and important working principles that is widely being put into practical applications. The thermoelectric property of semiconducting tin oxide film has been utilized in the sensor that has been developed. The thermoelectric property of semiconducting tin oxide film has been utilized in the sensor. The deposition parameters for sputtering of tin oxide film have been optimized to obtain a high seebeck coefficient. A test set-up to characterize the deposited films for their thermoelectric property has been designed and developed. A novel method of increasing the seebeck coefficient of tin oxide films has been successfully implemented. Thin films of chromium, copper and silver were used for this purpose. Deposition of the semiconducting oxide on strips of metal films has led to a noticeable increase in the seebeck coefficient of the oxide film without significantly affecting its thermal conductivity. The next part of our work involved development of a gas sensor using this thermoelectric film. These sensors were further tested for their response to volatile organic compounds. The sensor showed significant sensitivity to the test gases at relatively low temperatures. In addition to this, the developed sensor is also selective to acetone gas.