Influence of Pd-loading on gas sensing characteristics of SnO2 thick films

Nanocrystalline pristine and 0.5, 1.5 and 3.0 wt% Pd loaded SnO₂ were synthesized by a facile co-precipitation route. These powders were screen-printed on alumina substrates to form thick films to investigate their gas sensing properties. The crystal structure and morphology of different samples were characterized by using X-ray diffraction, scanning electron microscopy and transmission electron microscopy techniques. The 3.0 wt% Pd:SnO₂ showed response of 85% toward 100 ppm of LPG at operating temperature of 250 °C with fast response (8 s) and quick recovery time (24 s). The high response toward LPG on Pd loading can be attributed to lowering of crystallite size (9 nm) as well as the role of Pd particles in exhibiting spill-over mechanism on the SnO₂ surface. Also selectivity of 3.0 wt% Pd:SnO₂ toward LPG was confirmed by measuring its response to other reducing gases like acetone (CH₃COCH₃), ethanol (C₂H₅OH) and ammonia (NH₃) at optimum operating temperature.     

Highly sensitive acetone sensor based on Eu-doped SnO2 electrospun nanofibers

In this study, a series of undoped and Eu-doped SnO₂ nanofibers were synthesized via a simple electrospinning technique and subsequent calcination treatment. Field-emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) were carefully used to characterize the morphologies, structures and chemical compositions of these samples. The results reveal that the as-prepared nanofibers are composed of crystallite grains with an average size of about 10 nm and Eu³⁺ ions are successfully doped into the SnO₂ lattice. Compared with pure SnO₂ nanofibers, Eu-doped SnO₂ nanofibers demonstrate significantly enhanced sensing characteristics (e.g., large response value, short response/recovery time and outstanding selectivity) toward acetone vapor, especially, the optimal sensor based on 2 mol% Eu-doped SnO₂ nanofibers shows the highest response (32.2 for 100 ppm), which is two times higher than that of the pure SnO₂ sensor at an operating temperature of 280 °C. In addition, the sensor exhibits a good sensitivity to acetone in sub-ppm concentrations and the detection limit could extend down to 0.3 ppm, making it a potential candidate for the breath diagnosis of diabetes.     

Improved ethanediol sensing with single Yb ions doped SnO2 nanobelt

Yb-doped SnO₂ nanobelts (Yb–SnO₂ NBs) and pure SnO₂ nanobelts (SnO₂ NBs) are successfully synthesized by thermal evaporation method and their composition and morphology are characterized. The single nanobelt device is fabricated by dual-ion beam deposition system, and the gas sensing performance to ethanediol, methanal, ethanol and acetone is investigated. The results show that the best working temperature of single Yb–SnO₂ NB sensor to ethanediol is 190 °C, which is lower than that of pure counterpart and the highest sensitivity is 10.5 to 100 ppm of ethanediol. In addition, it is found that the response/recovery time is short and the sensor exhibits excellent selectivity and stability. The sensing performance of SnO₂ NB is actually improved by Yb.     

Tin–Zinc oxide composite ceramics for selective CO sensing

Composite metal oxide gas sensors were intensely studied over the past years having superior performance over their individual oxide components in detecting hazardous gases. A series of pellets with variable amounts of SnO₂ (0–50 mol%) was prepared using wet homogenization of the component oxides leading to the composite tin-zinc ceramic system formation. The annealing temperature was set to 1100 °C. The samples containing 2.5 mol% SnO₂ and 50 mol% SnO₂ were annealed also at 1300 °C, in order to observe/to investigate the influence of the sintering behaviour on CO detection. The sensor materials were morphologically characterized by scanning electron microscopy (SEM). The increase in the SnO₂ amount in the composite ceramic system leads to higher sample porosity and an improved sensitivity to CO. It was found that SnO₂ (50 mol%) - ZnO (50 mol%) sample exhibits excellent sensing response, at a working temperature of 500 °C, for 5 ppm of CO, with a fast response time of approximately 60 s and an average recovery time of 15 min. Sensor selectivity was tested using cross-response to CO, methane and propane. The results indicated that the SnO₂ (50 mol%)-ZnO (50 mol%) ceramic compound may be used for selective CO sensing applications.     

Essential Macleod Program (EMP) simulated fabrication of high quality Zn:SnO2/Ag/Zn:SnO2 multilayer transparent conducting electrode on flexible substrates

In the quest of promising Indium free amorphous transparent conducting oxide (TCO), Zn-doped SnO₂/Ag/Zn-doped SnO₂ (OMO) multilayer films were prepared on flexible polyethylene terephthalate (PET) substrates by RF sputtering at room temperature (RT). Growth parameters were optimized by varying sputtering power and working pressure, to have high electrical conductivity and optical transmittance. Optimization of the thickness of each layer was done by Essential Macleod Program (EMP) simulation to get the higher transmission through OMO multilayer. The sheet resistance and transmittance of 3 at% Zn-doped SnO₂ thin film (30 nm) were 2.23 kΩ/□, (ρ ~ 8.92×10⁻³ Ω∙cm) and 81.3% (at λ ~ 550 nm), respectively. By using optimized thicknesses of Zn-doped SnO₂ (30 nm) and Ag (12 nm) and optimized growth condition Zn-doped SnO₂/Ag/Zn-doped SnO₂ multilayer thin films were deposited. The low sheet resistance of 7.2 Ω/□ and high optical transmittance of 85.1% in the 550 nm wavelength region was achieved with 72 nm multilayer film.     

The effect of Sm2O3 on the microstructure and electrical properties of SiO2-doped SnO2-Zn2SnO4 ceramic varistors

In this work, Sm₂O₃- and SiO₂-codoped SnO₂-Zn₂SnO₄ ceramic varistors were prepared through traditional ceramic processing, and the effect of Sm₂O₃ on the resulting microstructure and electrical properties was investigated. The results demonstrated that the ceramics were composed mainly of SnO₂ and Zn₂SnO₄, and Sm was distributed homogeneously in the grains and along the grain boundaries. With 0.2 mol% Sm₂O₃ doping, the grain growth was obviously promoted. Further increases in Sm₂O₃ to 0.4 mol% resulted in trace amount of SiO₂ and segregations containing elemental Sm via X-ray diffraction patterns and microstructure photos, respectively. In the sample doped with 0.3 mol% Sm₂O₃, optimal electrical characteristics of α=9.4, E_B=10 V/mm, J_L=46 μA/cm² and ε′=1.2×10⁴ were obtained. Simultaneously, the sample doped with 0.3 mol% Sm₂O₃ had the lowest conductance activation energy of 0.16 eV at temperatures lower than 110 °C. This good performance indicates that Sm₂O₃- and SiO₂-codoped SnO₂-Zn₂SnO₄ composite ceramics are viable candidate for the manufacture of capacitor-varistor functional devices.     

Coal liquefaction with in situ impregnated Fe2(MoS4)3 bimetallic catalyst

Daliuta subbituminous coal (DL), loaded with Fe₂(MoS₄)₃ bimetallic catalyst, was liquefied in a 50 ml micro-autoclave with tetralin as solvent at 440 °C, initial hydrogen of 6.0 MPa, soaking time of 30 min in attempt to produce one to four ring aromatic chemicals. The catalytic effects of in situ impregnated Fe₂(MoS₄)₃ in water solution with and without surfactant were investigated in terms of coal conversion, oil+gas yield and the yields of aromatic, aliphatic and polar compound fractions in the oil. The conversion, oil+gas, aromatics and polar compound yields of DL coal, loaded with 1 wt% daf FeMo of Fe₂(MoS₄)₃ bimetallic catalyst, were 78.2, 70.5, 20.8 and 16.7 wt% daf, respectively, which were higher than those with 1.0 wt% Fe (based on daf coal) of Fe₂S₃ (62.6, 54.2, 13.4, 13.2 wt% daf, respectively) or 1.0 wt% Mo of ammonium tetrathiomolybdate (70.8, 63.2, 16.7, 14.1 wt% daf, respectively) alone under the same conditions. When the catalyst was impregnated on coal in surfactant solution, the coal conversion and product yields were further increased.     

Preparation by solar physical vapor deposition (SPVD) and nanostructural study of pure and Bi doped ZnO nanopowders

Pure and Bi doped ZnO nanopowders have been prepared by a physical vapor deposition process in a solar reactor (SPVD). From X-ray diffraction (XRD) spectra performed on initial targets and on the nanopowders obtained, the lattice parameters and the phase changes as well as the average grain sizes and the grain shape anisotropies have been determined. High Resolution Transmission Electron Microscopy (HRTEM) observations support the results. The pure ZnO nanopowders “grain size” and “grain shape anisotropy” (whiskers with an average diameter of 20–40 nm) is a function of the air pressure during the vaporisation–condensation process: the higher the pressure, the longer the whiskers. The bismuth doped ZnO nanopowders are polyphased but the ZnO based majority phases behave similarly to pure ZnO with a tendency to form whiskers but with a grain size and grain shape anisotropy decreasing when the Bi content increases.Preliminary electrical measurements at temperatures below 300 °C have shown that the ionic conductivity of the nanocomposites obtained starting from ZnO + 23 wt% Bi₂O₃ targets is high and promising for applications.     

Nanostructured SnO2 thin films for NO2 gas sensing applications

We report the synthesis of nanostructured SnO₂ by a simple inexpensive sol–gel spin coating method using m-cresol as a solvent. This method facilitates rapid synthesis at comparatively lower temperature enabling formation of nanostructures suitable for gas-sensing applications. Various physicochemical techniques have been used for the characterization of SnO₂ thin films. X-ray diffraction analysis confirmed the single-phase formation of tetragonal SnO₂ having crystallite size 5–10 nm. SnO₂ showed highest response (19%) with 77.90% stability toward 100 ppm nitrogen dioxide (NO₂) at 200 °C. The response time of 7 s and recovery time of 20 min were also observed with the same operating parameters. The probable mechanism is proposed to explain the selective response toward nitrogen dioxide. Impedance spectroscopy studies showed that the response to nitrogen dioxide is mainly contributed by grain boundaries. The reproducibility and stability study of SnO₂ sensor confirmed its candidature for detection of NO₂ gas at low concentration (10–100 ppm) and lower operating temperature.     

Synthesis of nanocrystalline cerium oxide by high energy ball milling

We have synthesized pure nanocrystalline CeO₂ powders of nearly spherical shape using high-energy attritor ball mill. Milling parameters such as the milling speed of 400 rpm, ball to powder ratio (40:1), milling time (30 h) and water cooled media were determined to be suitable for synthesizing nanosize (～10 nm) powders of CeO₂. The powders after milling for various durations (up-to 50 h) were characterized by X-ray Diffraction, Scanning Electron Microscopy, Energy-dispersive X-ray Spectrometry and Transmission Electron Microscopy. An average particle size of 10 nm was obtained at 30 h milling, after which the particle agglomeration started, and a mixture of nanocrystalline and amorphous phase was observed after 50 h milling.     

Enhanced gas sensing properties to NO2 of SnO2/rGO nanocomposites synthesized by microwave-assisted gas-liquid interfacial method

The detection of nitrogen dioxide (NO₂) is essential for the environment and human health. Tin dioxide (SnO₂) based sensors have demonstrated capabilities to detect NO₂, while their response, response/recover speed and selectivity are not good enough for their practical applications. To address these issues, the SnO₂ nanoparticles doped with reduced graphene oxides (rGO) have been synthesized by using a facile microwave-assisted gas-liquid interfacial solvothermal method in this work. The NO₂ sensing performances have been greatly enhanced after the doping of rGO due to the improved electronic conductivity and the formation of the p-n junction in the as-synthesized SnO₂/rGO nanocomposites. Moreover, our results demonstrate that the sensors based on the SnO₂/(0.3%)rGO nanocomposites (with an average diameter about 10–15 nm) exhibit the best overall performance with the high response of 247.8 to 10 ppm NO₂, fast response/recovery speed (39 s/15 s) and the excellent selectivity at the working temperature of 200 ℃. Remarkably, the SnO₂/(0.3%)rGO sensors still exhibit a good gas sensing performance to NO₂ even at room temperature.     

Effect of Pt or Pd doping on stability of TiO2 nanoparticle suspension in water

Stability of suspensions of TiO₂ nanoparticles synthesized by the flame aerosol reactor (FLAR) could be altered by doping TiO₂ nanoparticles with Pt, Pd, or Pt–Pd dopants. It was found that doping of TiO₂ with Pd or Pt could contribute to the control of the agglomeration of TiO₂ suspended in water. With the change of doping content, the isoelectric point (IEP) of stable TiO₂ suspension decreased gradually from 5 to 3.6 while the specific surface area was increased from 43.27 to 60.84 m²/g. With pH > 6.0, 2 wt% Pt–Pd/TiO₂ suspension exhibited the lowest agglomeration behavior. The plausible intrinsic structures of Pt, Pd, and Pt–Pd doped TiO₂ nanoparticles were proposed and discussed with respect to their IEP based on the DLVO theory.     

Enhanced gas sensing properties of hierarchical SnO2 nanoflower assembled from nanorods via a one-pot template-free hydrothermal method

Well-defined three-dimensional (3D) hierarchical tin dioxide (SnO₂) nanoflowers with the size of about 200 nm were successfully synthesized by a simple template-free hydrothermal method. X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and N₂ adsorption-desorption analyses were used to characterize the structure and morphology of the products. The as-synthesized full crystalline and large specific surface area SnO₂ nanoflowers were assembled by one-dimensional (1D) SnO₂ nanorods with sharp tips. A possible self-assembly mechanism for the formation the SnO₂ nanoflowers was speculated. Moreover, gas sensing investigation showed the sensor based on SnO₂ nanoflowers to exhibit high response and fast response-recovery ability to detect acetone and ethanol at an operating temperature lower than 200 °C. The enhancement of gas sensing properties was attributed to their 3D hierarchical nanostructure, large specific surface area, and small size of the secondary SnO₂ nanorods.     

Fabrication of SnO2/SnS2 hybrids by anchoring ultrafine SnO2 nanocrystals on SnS2 nanosheets and their photocatalytic properties

Ultrafine SnO₂ nanocrystals with sizes of ~4 nm have been successfully loaded on the SnS₂ nanosheets to fabricate SnO₂/SnS₂ hybrids via a facile hydrothermal method. The obtained samples are well characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), high resolution transmission electron microscopy (HRTEM), X-ray photoelectron spectroscopy (XPS), UV–vis spectroscopy, photoluminence (PL) and electrochemical impedance spectroscopy (EIS). The experimental results indicate that the SnO₂ nanocrystals of ~4 nm are well dispersed and intimately anchored on the SnS₂ nanosheets to form nanosized heterojunctions, which can be favorable to the separation of photo-generated holes and electrons. Consequently, the SnO₂/SnS₂ hybrids demonstrate obviously enhanced photocatalytic activities for reduction of Cr (VI) under visible light compared with both the bare SnO₂ and SnS₂.     

Preparation and characterization of polysulfone mixed matrix membrane incorporated with palladium nanoparticles in the inversed microemulsion for hydrogen separation

Polysulfone (PSf) membrane shows acceptable gas separation performance, but its application is limited by the “trade-off” between selectivity and permeability. In this study, PSf mixed matrix membranes (MMMs) incorporated with palladium (Pd) nanoparticles in the inversed microemulsion were proposed for hydrogen (H₂) separation. Pd nanoparticles can be kinetically stabilized and dispersed using electrostatic and/or steric forces of a stabilizer which is typically introduced during the formation of Pd nanoparticles in the inversed microemulsion. Pd nanoparticles were synthesized by loading (PdCl₂) into the polymeric matrix, polyethylene glycol (PEG) which acts as reducing agent and stabilizer. The dry–wet phase inversion method was applied for the preparation of asymmetric PSf MMMs. The effects of Pd (0–4 wt%) on the membrane characteristics and separation performance were studied. Experimental findings verified that the MMMs are able to achieved a high H₂/N₂ selectivity of 21.69 and a satisfactory H₂ permeance of 46.24 GPU due to the changes in membrane structure from fully developed finger-like structure to closed cell structure besides the growth of dense layer. However, the selectivity of H₂/CO₂ decreased due to the addition of PEG.     

Enhanced performance of γ-Fe2O3:WO3 nanocomposite towards selective acetone vapor detection

Metal oxide nanocomposite sensors based on γ-Fe₂O₃ and WO₃ were investigated in acetone vapor of various concentrations (1–100 ppm) at operating temperatures between 250 and 350 °C. The composites were prepared by simple solid state mixing and porous thick-film gas sensors were fabricated on alumina substrates. The γ-Fe₂O₃:WO₃ (50:50) nanocomposite showed a marked enhancement in sensing response down to 1 ppm acetone vapor detection at 300 °C. The response was ~2-fold better compared to pure WO₃ or pure γ-Fe₂O₃ with a very fast response (1 s) and very short recovery time (3 s). No appreciable sensitivity was observed towards alcohol vapor (an interfacing agent for diabetics) and in moisture (present in breath). The enhanced performance was due to n–n heterojunction effect.     

Fabrication and modification of cellulose acetate based mixed matrix membrane: Gas separation and physical properties

[Cellulose acetate (CA)-blend-multi walled carbon nano tubes (MWCNTs)] mixed matrix membranes (MMMs), [CA/polyethylene glycol (PEG)/MWCNTs] and [CA/styrene butadiene rubber (SBR)/MWCNTs] blend MMMs were prepared by solution casting method for gas separation applications using Tetrahydrofuran (THF) as solvent. Both raw-MWCNTs (R-MWCNTs) and functionalized carboxylic-MWCNTs (C-MWCNTs) were used in membrane preparation. The MWCNTs loading ratio and pressure effects on the gas separation performance of prepared membranes were investigated for pure He, N₂, CH₄ and CO₂ gases. Results indicated that utilizing C-MWCNT instead of R-MWCNTs in membrane fabrication has better performance and (CO₂/CH₄) and (CO₂/N₂) selectivity reached to 21.81 and 13.74 from 13.41 and 9.33 at 0.65 wt% of MWCNTs loading respectively. The effects of PEG and SBR on the gas transport performance and mechanical properties were also investigated. The highest CO₂/CH₄ selectivity at 2 bar pressure was reached to 53.98 for [CA/PEG/C-MWCNT] and 43.91 for [CA/SBR/C-MWCNT] blend MMMs at 0.5 wt% and 2 wt% MWCNTs loading ratio respectively. Moreover, increase of feed pressure led to membrane gas permeability and gas pair selectivity improvement for almost all prepared membranes. The mechanical properties analysis exhibited tensile modules improvement with increasing MWCNTs loading ratio and utilizing polymer blending.     

Transparent gas senor and photodetector based on Al doped ZnO nanowires synthesized on glass substrate

In this work high density, well-aligned Al doped ZnO (AZO) nanowires are hydrothermally synthesized on glass substrate at 99 °C. The Al content is ~1.57 at%. The PL spectrum shows that Al impurities caused an increase in the number of oxygen vacancies. The spectral response results show that the maximum responsivity and quantum efficiencies η of AZO NWs are 3.61 A/W and 84.9%, at an incident light wavelength of 360 nm. These AZO NWs have less humidity sensitivity, thus decreasing the effect of humidity effect on gas sensing. Low gas concentrations of 10 ppm ethanol and 10 ppm acetone can be detected with good responses of 24.5% and 21.2%, using the AZO NW sensor at 200 °C and with 0.1 V applied bias.     

Selective epoxidation of styrene with air catalyzed by CoOx and CoOx/SiO2 without any reductant

Cobalt oxide (CoOx) prepared by a direct calcination of cobalt nitrate was considerably active for the epoxidation of styrene with air in DMF under mild conditions. A substrate conversion of 75.8 mol% with an epoxide selectivity of 82.1% was achieved at 353 K over 10 mg of cobalt oxide catalyst. Once CoOx was loaded on the support SiO₂ through a simple procedure consisting of wet impregnation, drying and calcination, the as-prepared catalyst presented higher catalytic activity and epoxide selectivity than cobalt oxide itself. Over the optimized catalyst CoOx/SiO₂ (1.0 wt% Co), 85.7 mol% of styrene was effectively converted at 363 K within 4 h, with a high epoxide selectivity up to 86.0%. The results showed that many factors influenced the performance of the catalyst, such as the Co loading, the support, the temperature and the atmosphere, etc. The leaching of cobalt from the catalyst CoOx/SiO₂ was negligible, indicating the applicability of the catalyst CoOx/SiO₂ as a true heterogeneous catalyst. The control test and UV–vis spectra revealed a synergic interaction among solvent, oxygen and substrate over CoOx/SiO₂.     

New 3D stratified Si-Ca-P porous scaffolds obtained by sol-gel and polymer replica method: Microstructural,mineralogical and chemical characterization

The aim of this research was to develop and characterize a novel stratified porous scaffold for future uses in bone tissue engineering. In this study, a calcium silicophosphate porous scaffold, with nominal composition 29.32 wt% SiO₂ – 67.8 wt% CaO – 2.88 wt% P₂O₅, was produced using the sol-gel and polymer replication methods. Polyurethane sponges were used as templates which were impregnated with a homogeneous sol solution and sintered at 950 °C and 1400 °C during 8 h. The characteristics of the 3D stratified porous scaffolds were investigated by Scanning Electron Microscopy, X-Ray Diffraction, Fourier Transform Infrared Spectrometry, Diametric Compression of Discs Test and Hg porosimetry techniques. The result showed highly porous stratified calcium silicophosphate scaffolds with micro and macropores interconnected. Also, the material has a diametrical strength dependent on the number of layers of the stratified scaffolds and the sintering temperature.