Synthesis of indium oxide cubic crystals by modified hydrothermal route for application in room temperature flexible ethanol sensors

Indium oxide cubic crystals were prepared by using hexamethylenetetramine and indium chloride without the addition of any structure directing agents. The chemical route followed in the present work was a modified hydrothermal synthesis. The average crystallite size of the prepared cubes was found to be 40 nm. A blue emission at 418 nm was observed at room temperature when the sample was excited with a 380 nm Xenon lamp. This emission due to oxygen vacancies made the material suitable for gas sensing applications. The synthesized material was made as a composite film with polyvinyl alcohol which was more flexible than the films prepared on glass substrates. This flexible film was used as a sensing element and tested with ethanol vapours at room temperature. The film showed fast response as well as recovery to ethanol vapours with a sensor response of about 1.4 for 100 ppm of the gas.     

Effect of In incorporation on the structural, electrical, and gas sensing properties of ZnO films

In this paper, we report some comparative results on the structural, electrical, and gas sensing properties of undoped, In-doped ZnO, and ZnO–In₂O₃ thin films, respectively. The oxide films were obtained by thermal oxidation (flash oxidation) of metallic films, deposited by thermal evaporation under vacuum. X-ray diffraction patterns reveal that oxidized films are polycrystalline, the crystallites being preferentially oriented with (002) planes parallel with the substrate. It was observed that the films’ morphology, investigated by atomic force microscopy and scanning electron microscopy, is influenced by the In amount. The temperature dependence of electrical conductivity was studied and obtained results indicate that In-doped ZnO and ZnO–In₂O₃ films exhibit an enhancement of electrical conductivity with four orders of magnitude by comparison with undoped ZnO film. Gas sensitivity measurements were performed for four different gases (ammonia, methane, acetone, and ethanol), and it was observed that all investigated films are more sensitive to ammonia. Also, it was observed that gas sensitivity is visibly increased for In-doped ZnO and ZnO–In₂O₃ samples by comparison with undoped ZnO film.     

Structural,morphological, optical and gas sensing properties of pure and Ce doped SnO<Subscript>2</Subscript> thin films prepared by jet nebulizer spray pyrolysis (JNSP) technique

Pure and cerium (Ce) doped tin oxide (SnO₂) thin films are prepared on glass substrates by jet nebulizer spray pyrolysis technique at 450 °C. The synthesized films are characterized by X-ray diffraction (XRD), scanning electron microscopy, energy dispersive analysis X-ray, ultra violet visible spectrometer (UV–Vis) and stylus profilometer. Crystalline structure, crystallite size, lattice parameters, texture coefficient and stacking fault of the SnO₂ thin films have been determined using X-ray diffractometer. The XRD results indicate that the films are grown with (110) plane preferred orientation. The surface morphology, elemental analysis and film thickness of the SnO₂ films are analyzed and discussed. Optical band gap energy are calculated with transmittance data obtained from UV–Visible spectra. Optical characterization reveals that the band gap energy is found decreased from 3.49 to 2.68 eV. Pure and Ce doped SnO₂ thin film gas sensors are fabricated and their gas sensing properties are tested for various gases maintained at different temperature between 150 and 250 °C. The 10 wt% Ce doped SnO₂ sensor shows good selectivity towards ethanol (at operating temperature 250 °C). The influence of Ce concentration and operating temperature on the sensor performance is discussed. The better sensing ability for ethanol is observed compared with methanol, acetone, ammonia, and 2-methoxy ethanol gases.     

Ethanol and LPG sensing characteristics of SnO<Subscript>2</Subscript> activated Cr<Subscript>2</Subscript>O<Subscript>3</Subscript> thick film sensor

The sensing response of pure and SnO₂ activated Cr₂O₃ to ethanol vapours and liquefied petroleum gas (LPG) has been investigated. Fine particles of commercial chromium oxide powder were selected and deposited as thick film to act as a gas sensor. The sensor surface has been activated by tin dioxide, on surface oxidation of tin chloride. The concentration of tin chloride solution, used as activator, was varied from 0 to 5% and its effect on gas response, selectivity and operating temperature has been studied. It was found that response to ethanol vapours significantly improved, whereas response to LPG remained unaffected. Moreover, operating temperature remains unchanged both for LPG and ethanol vapours.     

Thin polyaniline and polyaniline/carbon nanocomposite films for gas sensing

We have studied the gas sensing properties of five polyaniline-based materials—thick and thin PANI films, nanocomposite PANI/MWNT and PANI/SWNT films, and PANI nanogranules embedded in a polyvinylpyrrolidone matrix. The films (except for the latter) were deposited within the induction period of the polymerization process on gold interdigitated micro electrodes. Their sensitivity to NH₃, H₂, ethanol, methanol, and acetone was measured. The thin PANI film (~ 100 nm thick) prepared by a lift-off process had the sensitivity to ammonia below 0.5 ppm, which was higher than that of nanocomposite films. Two materials—thick PANI film and nanocomposite PANI/MWNT film—exhibited a shallow minimum in the temperature dependence of resistance (at 313 K and 319 K), which is a feature exploitable in practical applications, since the gas sensors should be insensitive to small temperature fluctuations at these temperatures.     

Effect of air-pressure on room temperature hydrogen sensing characteristics of nanocrystalline doped tin oxide MEMS-based sensor

Nanocrystalline indium oxide (In2O3)-doped tin oxide (SnO2) thin film sensor has been sol-gel dip-coated on a microelectrochemical system (MEMS) device using a sol-gel dip-coating technique. Hydrogen (H2) at ppm-level has been successfully detected at room temperature using the present MEMS-based sensor. The room temperature H2 sensing characteristics (sensitivity, response and recovery time, and recovery rate) of the present MEMS-based sensor has been investigated as a function of air-pressure (50-600 Torr) with and without the ultraviolet (UV) radiation exposure. It has been demonstrated that, the concentration of the surface-adsorbed oxygen-ions (which is related to the sensor-resistance in air), the ppm-level H2, and the oxygen (O2) partial pressure are the three major factors, which determine the variation in the room temperature H2 sensing characteristics of the present MEMS-based sensor as a function of air-pressure.     

氧化锡纳米线的制备及其乙醇气体敏感性能

采用热蒸发法成功制备氧化锡纳米线。用X射线衍射、扫描电子显微镜和透射电子显微镜对所制备纳米线的晶格结构和表面形貌进行表征。所制材料为金红石氧化锡单晶结构,纳米线直径为50~200nm,长度为5~15μm,符合气-液-固生长机制。以氧化锡为气敏材料,制备了旁热式结构气敏元件,测试该元件对浓度范围为25×10^-6 ~500×10^-6 的乙醇气体环境的敏感性能。结果表明,该元件的最佳工作温度约为260℃;在25×10^-6 和500×10^-6 的乙醇气体中,灵敏度分别为7.54和111.01,响应时间为2~20s,恢复时间为5~33s;在测试范围内灵敏度与气体浓度具有良好的线性关系;7天内重复测量误差在5%以内,稳定性较好。     

电子束低温蒸发ITO膜增透、增反特性研究

本实验是在低温条件下，采用电子柬蒸发制备ITO透明导电薄膜，通过监测电阻来控制薄膜的厚度，通过控制薄膜厚度研究了增透和增反两种效果的ITO膜的制备及膜的光学特性。当膜厚达170nm和83nm时透过率和反射率可达95％和6％。     

Structural, optical and gas sensing properties of spin coated nanocrystalline zinc oxide thin films

Synthesis of nanocrystalline zinc oxide thin films by sol gel spin coating technique and its application as ammonia gas sensor is presented in this paper. The synthesized sample is pure zinc oxide with hexagonal wurtzite structure. The lattice parameters are: a = 3.2568 Å and c = 5.210 Å. Average crystallite size is of the order of 58 nm. SEM studies show that growth of the film takes place with folded structure, increasing the open surface area of the film. Optical study revealed that band gap of ZnO is 3.25 eV with direct band to band transitions. Gas sensing characteristics showed that ZnO film is sensitive as well as fast responding to ammonia gas at 573 K. A high sensitivity for ammonia gas indicates that the ZnO films are selective for this gas. The rise time and recovery time are 25 and 80 s, respectively. The mechanism of gas sensing is explained adequately.     

Microsensor based on low temperature cofired ceramics and gas-sensitive thin film

A novel design of gas sensor using low temperature cofired ceramics (LTCC) and thin film technologies is presented. The LTCC structure is composed essentially of two ceramic layers with interlayer thick film Pt heater, interdigitated electrodes on top, contact pads and metallic connections realised by vias. The thin films of both SnO₂ and In₂O₃, intentionally doped and activated, were deposited on top of the structure. With some modifications of the lamination process and heat treatment parameters, the authors obtained the upper ceramic layer with the roughness not exceeding 250 nm, what was suitable for thin film technology. The films deposited onto such LTCC structure revealed the sensing properties very similar to the reference films deposited onto glass. The gas-sensitive films were tested with changing concentrations of reducing and oxidising gases in air. The necessary sensor working temperature was obtained and stabilised using a custom-built digital controller. The low heat capacity of the sensor structure enabled also a sinusoidal temperature control. The satisfactory results obtained by the authors indicate that the connection of LTCC and thin film technologies can lead to the fabrication of good quality gas sensors.     

Fabrication and characterization of nanostructured indium tin oxide film and its application as humidity and gas sensors

This paper reports the synthesis and characterization of nanocrystalline indium tin oxide (ITO) and its application as humidity and gas sensors. The structure and crystallite size of the synthesized powder were determined by X-ray diffraction. The minimum crystallite size was found 5 nm by Debye–Scherrer equation and confirmed by transmission electron microscopy image. Optical characterizations of ITO were studied using UV–visible absorption spectroscopy and Fourier transforms infrared spectroscopy. Thermal analysis was carried out by differential scanning calorimetry. Further, the ITO thin film was fabricated using sol–gel spin coating method. The surface morphology of the fabricated film was investigated using scanning electron microscopy images. For the study of humidity sensing, the thin film of ITO was exposed with humidity in a controlled humidity chamber. The variations in resistance of the film with relative humidity were observed. The average sensitivity of the humidity sensor was found 0.70 MΩ/%RH. In addition, we have also investigated the carbon dioxide (CO₂) and liquefied petroleum gas sensing behaviour of the fabricated film. Maximum sensitivity of the film was ~17 towards CO₂. Its response and recovery times were ~5 and 7 min respectively. Sensor based on CO₂ is 97 % reproducible after 3 months of its fabrication. Better sensitivity, small response time and good reproducibility recognized that the fabricated sensor is challenging for the detection of carbon dioxide.     

Tungsten Oxide Thin Film Characterizations for Acetone Gas Detection

The gas sensing properties and topology of tungsten oxide thin films deposited by reactive-ion radio frequency magnetron sputtering at room temperature have been investigated. The abnormalities in behaviour of sensing film are observed when acetone gas is flowed over surface. The reduction reaction of surface and oxidation reaction of acetone gas have been studied. As the gas comes in contact with the surface, the molecules tend to reduce the surface, hence decreasing the resistance. The sensing film was annealed to 500 °C for 1 h for the purpose of achieving a suitable grain size for sensing to take place. Operational optimum temperature for sensing has been computed to be 260 °C. A grain size of 7.3 nm has been computed through analysis of AFM image and a film thickness of 100 nm has been calculated through surface profiler. The SEM image of the film demonstrates the grains developed on the surface. The XRD patterns reveal that the oxide showed up as WO₂. It has been observed that the response percentage is approximately 30% for acetone vapour concentration of 20 ppm and approximately 18% for the concentration of 15 ppm. The response time of the sensor is approximately 5 min and the recovery time is 4 min.     

Indium Tin Oxide Thin-Film Sensor for Detection of Volatile Organic Compounds (VOCs)

Indium tin oxide (ITO) (In₂O₃ + 17% SnO₂) thin films were grown on glass substrate by direct evaporation method. Two thick gold pads were deposited to take out contacts. The response of these films at different operating temperatures, when exposed to various volatile organic compounds (VOCs) such as methanol, ethanol, butanol, and acetone in the concentration range 200-2500 ppm was evaluated. Additionally, the effect of film thickness on the response charateristics of methanol and acetone was studied. The linearity and sensitivity of the sensors were measured. The ITO thin-film sensors showed a sensitivity of 0.256 ohms/ppm to acetone vapors, which was almost linear in the range 200-2500 ppm. In order to improve sensitivity and selectivity, a thin layer of various metal and metal oxides such as Cu and PbO was deposited on the sensor surface to work as catalytic layer and the effect on the performance of the sensor was studied. The response and recovery times of the sensor were determined for acetone vapors and were found to be 155 sec and 110 sec, respectively.     

Indium Tin Oxide thin film gas sensors for detection of ethanol vapours

Indium Tin Oxide (ITO: In₂O₃ + 17% SnO₂) thin films grown on alumina substrate at 648 K temperatures using direct evaporation method with two gold pads deposited on the top for electrical contacts were exposed to ethanol vapours (200-2500 ppm). The operating temperature of the sensor was optimized. The sensitivity variation of films having different thickness was studied. The sensitivity of the films deposited on Si substrates was studied. The response of the film with MgO catalytic layer on sensitivity and selectivity was observed. A novel approach of depositing thin stimulating layer of various metals/oxides below the ITO film was tried and tested.     

The influence of precursor powders and processing parameters on the properties of SnO2-based gas sensors

Semiconducting tin oxide precursor powders were synthesized via three different chemical processing routes. The influence of powder processing conditions on the physical properties, e.g., particle size, surface area and phase composition of both uncalcined and calcined materials, was investigated. These powders were used to fabricate gas sensors using thick-film screen-printing technology. The effect of precursor powders, sintering conditions, sensor temperature and Pd catalyst on the carbon monoxide, methane, propane and ethanol gas sensing characteristics of the sensors were investigated. Sensors were also fabricated using tin oxide powders obtained from a commercial source and their gas sensing properties were also investigated. The data indicates that the powder processing methodology, sensor fabrication conditions and Pd catalyst can profoundly influence the physical characteristics as well as the gas sensing properties of the sensors.     

In2O3基酒敏材料的催化及气敏性能

采用微反-气相色谱联用装置和气敏性能测试设备,系统评价了不同粒径、不同掺杂的Ia2O3材料对乙醇的催化、气敏性能.研究表明,采用纳米材料可将乙醇灵敏度由6.0提高到16.0,掺杂碱性金属氧化物将灵敏度提高到14.0;掺杂贵金属可大幅度提高材料对乙醇的催化活性,但降低对乙醇的灵敏度.材料的气敏性能和催化性能存在密切的联系,浅析了材料对乙醇的敏感机理.     

Sterically hindered phthalocyanines: solid-phase interactions with carbon monoxide in matrix-entrapped thin functional films

A thin film comprising highly sterically hindered iron phthalocyanine derivatives incorporated into sol–gel networks shows effective sensitivity to carbon monoxide gas, when monitored by UV–visible absorption spectroscopy at 670 nm. The absorbance of a sol–gel thin film incorporating octaphenyl-di-tert-butylphthalocyanine iron(II) was particularly sensitive to carbon monoxide gas and showed a change in absorption after exposure to 1000 ppm CO gas for 1 min, while repetitive exposures produced only a limited loss of response. The optical response of the thin film gradually decreases with increasing temperature, and the binding energy for this sensing phenomenon was calculated to be 0.401 eV. The spectrum recovers at room temperature some 5 min after exposure to the gas.     

Effect of rf power on the structural properties of indium tin oxide thin film prepared for application in hydrogen gas sensor

Indium tin oxide films were grown on glass substrate by rf magnetron sputtering at 648 K. Influence of rf power on structural properties of the ITO films was studied. XRD measurements showed (222) preferred orientation under the optimized deposition conditions. The surface morphology of ITO films analyzed by scanning electron microscope appears to be uniform over the entire surface area, the film exhibited dense layers with fine grains. Finally, ITO sensor device was fabricated and the sensing properties of the device towards hydrogen gas were investigated. The variation in sensitivity of the ITO sensor with operating temperature and with concentration of hydrogen gas was studied. The maximum response was found to be 1.6 at 400 K, for 1,000 ppm of hydrogen gas, and the response of the sensor was found to decrease with increase in concentration of H₂ gas.     

Low temperature deposition of indium tin oxide films by plasma ion-assisted evaporation

Coatings of transparent conductive oxides, especially indium tin oxide (ITO), are important in different fields. So far, application of these materials has been limited to substrates with high thermal stability. We describe an improved coating process for ITO based on plasma ion-assisted evaporation at a substrate temperature below 100 degrees C, which is suitable for organic substrates. In characterizing the thin films, we used the classical Drude theory to calculate the resistivity from optical film properties and compared the data with linear four-point measurements. X-ray diffraction spectroscopy was used to determine the structural properties of the thin films.