Low-temperature CO gas sensors based on Au/SnO2 thick film

A study on the low-temperature CO gas sensors based on Au/SnO₂ thick film was reported. Au/SnO₂ powders were prepared by a deposition-precipitation method. Thick films were fabricated from Au/SnO₂ powders. X-ray diffraction (XRD), high-resolution transmission electron microscopy (HRTEM) and X-ray photoelectron spectroscopy (XPS) analyses were carried out for investigation of morphology and crystalline structure. Au/SnO₂ thick film sensors exhibited high sensitivity to CO gas at relatively low operating temperature (83-210 °C). We also reported the effect of the calcination temperature of Au/SnO₂ on the CO gas sensing behavior. The optimal calcination temperature of Au/SnO₂ was 300 °C.     

Fabrication of porous BaSnO3 hollow architectures using BaCO3@SnO2 core-shell nanorods as precursors

We present a strategy to synthesize porous BaSnO₃ hollow architectures with that were 150-300 nm in diameter and 1.5-5 μm in length using precursor of BaCO₃@SnO₂ nanorods prepared by hydrothermal treatment. BaCO₃@SnO₂ nanorods, consisting of a BaCO₃ core and a SnO₂ shell, could be used effectively for the solid-state synthesis of polycrystalline BaSnO₃ powder at 800 °C (lower than convention for BaCO₃ and SnO₂ mixtures). The core/shell structure of the precursor could play a role as a structural directing template for preparing BaSnO₃ hollow architectures during the calcination process. The X-ray diffractometer (XRD), scanning electron microscope (SEM), and transmission electron microscope (TEM) are employed to characterize the structures and morphologies. When applied to DSSC, the porous BaSnO₃ hollow architectures exhibit distinct photovoltaic effect.     

Effects of deposition temperature on the structural and morphological properties of SnO2 films fabricated by pulsed laser deposition

Tin oxide (SnO₂) thin films were grown on Si (1 0 0) substrates using pulsed laser deposition (PLD) in O₂ gas ambient (10 Pa) and at different substrate temperatures (RT, 150, 300 and 400 °C). The influence of the substrate temperature on the structural and morphological properties of the films was investigated using X-ray diffraction (XRD), atomic force microscopy (AFM) and scanning electron microscopy (SEM). XRD measurements showed that the almost amorphous microstructure transformed into a polycrystalline SnO₂ phase. The film deposited at 400 °C has the best crystalline properties, i.e. optimum growth conditions. However, the film grown at 300 °C has minimum average root mean square (RMS) roughness of 3.1 nm with average grain size of 6.958 nm. The thickness of the thin films determined by the ellipsometer data is also presented and discussed.     

Preparation and luminescence properties of Tb doped ZrO2 and BaZrO3 phosphors

ZrO₂:Tb³⁺ and BaZrO₃:Tb³⁺ powders are prepared by combustion synthesis method and the samples were further heated to 500, 700 and 1000 °C to improve the crystallinity of the materials. The structure and morphology of materials have been examined by X-ray diffraction, Raman spectra and scanning electron microscopy. It is remarkable that all the samples of ZrO₂:Tb³⁺ and BaZrO₃:Tb³⁺ have similar morphology. These images exhibited homogeneous aggregates of varying shapes and sizes, which are composed of a large number of small cuboids and broken cuboids. The cuboids and broken cuboids size of all the samples are less than 0.5 μm. Photoluminescence for both materials increases with increase of temperature and found maximum for the samples heated to 1000 °C with 5 mole% doping of Tb³⁺ ions. Luminescence is almost double for the zirconia compared to that of barium-zirconate.     

Influence of deposition temperature on the structural and morphological properties of Be3N2 thin films grown by reactive laser ablation

Be₃N₂ thin films have been grown on Si(1 1 1) substrates using the pulsed laser deposition method at different substrate temperatures: room temperature (RT), 200 °C, 400 °C, 600 °C and 700 °C. Additionally, two samples were deposited at RT and were annealed after deposition in situ at 600 °C and 700 °C. In order to obtain the stoichiometry of the samples, they have been characterized in situ by X-ray photoelectron (XPS) and reflection electron energy loss spectroscopy (REELS). The influence of the substrate temperature on the morphological and structural properties of the films was investigated using scanning electron microscopy (SEM), atomic force microscopy (AFM) and X-ray diffraction (XRD). The results show that all prepared films presented the Be₃N₂ stoichiometry. Formation of whiskers with diameters of 100-200 nm appears at the surface of the films prepared with a substrate temperature of 600 °C or 700 °C. However, the samples grown at RT and annealed at 600 °C or 700 °C do not show whiskers on the surface. The average root mean square (RMS) roughness and the average grain size of the samples grown with respect the substrate temperature is presented. The films grown with a substrate temperature between the room temperature to 400 °C, and the sample annealed in situ at 600 °C were amorphous; while the αBe₃N₂ phase was presented on the samples with a substrate temperature of 600 °C, 700 °C and that deposited with the substrate at RT and annealed in situ at 700 °C.     

SnO2微纳米材料的合成及其生长机理研究

利用简单的化学气相沉积法,以Sn粉为源材料合成不同形貌的一维SnO₂纳米棒、纳米线和纳米花等纳米结构,并通过减小载气中的氧含量获得新颖的SnO₂亚微米环状结构.通过调节Sn粉的量和载气中的氧含量、升温速率等试验条件,有效实现SnO₂一维纳米结构的控制生长.采用扫描电子显微镜、能谱仪和X射线衍射仪表征产物形貌、成分和物相结构,并探讨了SnO₂微纳米材料的生长机理. 关键词： 2')" href="#">SnO₂ 纳米结构 亚微米环 生长机理     

Microwave-assisted synthesis of SrFe12O19 hexaferrites

Ultra-fine and homogeneous SrFe₁₂O₁₉ hexaferrites were synthesized by a microwave-assisted calcination route. The calcined precursors were prepared by a sol-gel auto-combustion method using Fe(NO₃)₃·9H₂O, Sr(NO₃)₂ and citric acid as starting materials. The structures, powder morphology and magnetic properties of the products were characterized by X-ray diffraction, scanning electron microscope and vibrating sample magnetometer. The results showed that microwaves are helpful to reduce the calcination temperature and shorten the calcination time. The ferrites with saturation magnetization, remanence and intrinsic coercivity of 54.80 emu/g, 29.52 emu/g and 5261 Oe, respectively, were obtained in samples calcined at 800 °C for 80 min.     

Chemical synthesis of nanocrystalline SnO2 thin films for supercapacitor application

Nanocrystalline SnO₂ thin films were deposited by simple and inexpensive chemical route. The films were characterized for their structural, morphological, wettability and electrochemical properties using X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy techniques (SEM), transmission electron microscopy (TEM), contact angle measurement, and cyclic voltammetry techniques. The XRD study revealed the deposited films were nanocrystalline with tetragonal rutile structure of SnO₂. The FT-IR studies confirmed the formation of SnO₂ with the characteristic vibrational mode of Sn-O. The SEM studies showed formation of loosely connected agglomerates with average size of 5-10 nm as observed from TEM studies. The surface wettability showed the hydrophilic nature of SnO₂ thin film (water contact angle 9°). The SnO₂ showed a maximum specific capacitance of 66 F g⁻¹ in 0.5 Na₂SO₄ electrolyte at 10 mV s⁻¹ scan rate.     

CO sensor derived from mesostructured Au-doped SnO2 thin film

Pure and Au-doped mesostructured SnO₂ thin films were successfully prepared by using non-ionic surfactant Brij-58 (polyoxyethylene acyl ether) as organic template and tin tetrachloride and hydrogen tetrachloroaurate(III) trihydrate as inorganic precursor. Thin films were deposited onto the glass substrates at 450 °C by simple spray pyrolysis technique. The novel mesostructured tin oxide thin films with different Au concentration exhibit highly selective response towards CO. The correlation of the Au incorporation in the mesostructure with particular morphology and gas sensing behavior is discussed using scanning electron microscopy (SEM), X-ray diffraction (XRD), BET surface area and transmission electron microscopy (TEM) studies.     

Sol-gel growth of Gd2MoO6:Eu nanocrystalline layers on SiO2 spheres (SiO2@Gd2MoO6:Eu) and their luminescent properties

SiO₂@Gd₂MoO₆:Eu³⁺ core-shell phosphors were prepared by the sol-gel process. X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), field emission scanning electron microscopy (FESEM), energy-dispersive X-ray spectra (EDS), transmission electron microscopy (TEM), photoluminescence (PL) spectra as well as kinetic decays were used to characterize the resulting SiO₂@Gd₂MoO₆:Eu³⁺ core-shell phosphors. The XRD results demonstrate that the Gd₂MoO₆:Eu³⁺ layers on the SiO₂ spheres begin to crystallize after annealing at 600 °C and the crystallinity increases with raising the annealing temperature. The obtained core-shell phosphors have a near perfect spherical shape with narrow size distribution (average size ca. 600 nm), are not agglomerated, and have a smooth surface. The thickness of the Gd₂MoO₆:Eu³⁺ shells on the SiO₂ cores could be easily tailored by varying the number of deposition cycles (50 nm for four deposition cycles). The Eu³⁺ shows a strong PL luminescence (dominated by ⁵D₀-⁷F₂ red emission at 613 nm) under the excitation of 307 nm UV light. The PL intensity of Eu³⁺ increases with increasing the annealing temperature and the number of coating cycles.     

Preparation and photoluminescence characteristics of Eu-doped MgAl1.8Y0.2O4 nanocrystals

A simple combustion route was employed for the preparation of Eu³⁺-doped MgAl_1.8Y_0.2−xO₄ nanocrystals using metal nitrates as precursors and urea as a fuel in a preheated furnace at 500 °C. The powders thus obtained were then fired at 1000 °C for 3 h to get better luminescent properties. The incorporation of Eu³⁺ activator in these nanocrystals was checked by luminescence characteristics. These nanocrystals displayed bright red color on excitation under 254 nm UV source. The main emission peak was assigned to the transition [⁵D₀→⁷F₂] at 615 nm. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) studies were carried out to understand surface morphological features and the particle size. Crystal structures of the nanocrystals were investigated by the X-ray diffraction (XRD) technique. The crystallite size of the as-prepared nanocrystals was around 29 nm, which was evaluated from the broad XRD peaks. The crystallite size increased to ∼45 nm on further heat treatment at 1000 °C.     

Synthesis and magnetic properties of hard magnetic (CoFe2O4)-soft magnetic (Fe3O4) nano-composite ceramics by SPS technology

CoFe₂O₄/Fe₃O₄ nano-composite ceramics were synthesized by Spark Plasma Sintering. The X-ray diffraction patterns show that all samples are composed of CoFe₂O₄ and Fe₃O₄ phases when the sintering temperature is below 900 °C. It is found that the magnetic properties strongly depend on the sintering temperature. The two-step hysteresis loops for samples sintered below 500 °C are observed, but when sintering temperature reaches 500 °C, the step disappears, which indicates that the CoFe₂O₄ and Fe₃O₄ are well exchange coupled. As the sintering temperature increases from 500 to 800 °C, the results of X-ray diffractometer indicate the constriction of crystalline regions due to the ion diffusion at the interfaces of CoFe₂O₄/Fe₃O₄ phases, which have great impact on the magnetic properties.     

Gd-doped SnO2 nanoparticles: Structure and magnetism

Gd-doped SnO₂ nanoparticles were chemically prepared doping 0-12.5% Gd into SnO₂ and calcined at 600 °C. X-ray diffraction and Fourier transformed infrared spectroscopy measurements show the formation of single phase of Sn_1−xGd_xO₂ up to x=0.0625 while at x=0.125, an additional secondary phase of tetragonal GdO₂ (not cubic Gd₂O₃) is detected. The transmission electron microscopy studies show that the individual particles are single crystalline with an average size in the range of 10-12 nm. Magnetization measurements show the absence of ferromagnetic and antiferromagnetic ordering in all samples; however surface spin effects and enhanced Gd-O-Gd interactions are proposed to account for the observed magnetic properties of the samples.     

Thermal stability of HfO2 nanotube arrays

Thermal stability of highly ordered hafnium oxide (HfO₂) nanotube arrays prepared through an electrochemical anodization method in the presence of ammonium fluoride is investigated in a temperature range of room temperature to 900 °C in flowing argon atmosphere. The formation of the HfO₂ nanotube arrays was monitored by current density transient characteristics during anodization of hafnium metal foil. Morphologies of the as-grown and post-annealed HfO₂ nanotube arrays were analyzed by powder X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). Although monoclinic HfO₂ is thermally stable up to 2000 K in bulk, the morphology of HfO₂ nanotube arrays degraded at 900 °C. A detailed X-ray photoelectron spectroscopy (XPS) study revealed that the thermal treatment significantly impacted the composition and the chemical environment of the core elements (Hf and O), as well as F content coming from the electrolyte. Possible reasons for the degradation of the nanotube at high temperature were discussed based on XPS study and possible future improvements have also been suggested. Moreover, dielectric measurements were carried out on both the as-grown amorphous film and 500 °C post-annealed crystalline film. This study will help us to understand the temperature impact on the morphology of nanotube arrays, which is important to its further applications at elevated temperatures.     

Nanocoral architecture of TiO2 by hydrothermal process: Synthesis and characterization

TiO₂ thin films with novel nanocoral-like morphology were successfully grown directly onto the glass and conducting fluorine doped tin oxide coated glass substrates via multi-step hydrothermal (MSH) process. Titanium chloroalkoxide [TiCl₂ (OEt)₂ (HOEt)₂)] precursor was used in an aqueous saturated NaCl in presence of 1 mM HCl catalyst and HNO₃ peptizer at 120 °C. Reaction time varied from 3 to 12 h. The morphological features and physical properties of TiO₂ films were investigated by field emission scanning electron microscopy, high resolution transmission electron microscopy, X-ray diffraction, Fourier transform IR spectroscopy, Fourier transform Raman spectroscopy, room temperature photoluminescence spectroscopy and X-ray photoelectron spectroscopy. The surface morphology revealed the formation of TiO₂ corals having nanosized (30-40 nm) polyps. The photoelectrochemical properties of the TiO₂ nanocoral electrodes were investigated in 0.1 M NaOH electrolyte under UV illumination. The results presented in this study highlight two major findings: (i) ability to tune the photoelectrochemical response and photoconversion efficiency via controlled thickness of TiO₂ nanocorals and (ii) the substantial increase in short circuit photocurrent (J_sc) due to the improved charge transport through TiO₂ nanocorals prepared via MSH process. This approach would be quite useful for the fabrication of nanocoral architecture that finds key applications in photocatalysis, dye-sensitized solar cells and hybrid solar cells.     

Porous WO3 from anodized sputtered tungsten thin films for NO2 detection

In this paper, porous WO₃ films were prepared by anodic oxidation of metallic tungsten (W) films deposited on alumina substrates. The structural and morphological properties of the porous WO₃ films were investigated using field emission scanning electron microscope (FESEM) and X-ray diffraction (XRD). A large number of cracks appeared on the surface of films after anodization, which makes the films porous. The porous WO₃ sensors achieved their maximum response values to NO₂ at a low operating temperature of 150 °C. The porous WO₃ sensors showed high response values, great stability and fast response-recovery characteristics to different concentration of NO₂ gas due to the high specific surface area and special structural and morphological properties.     

Structural and optical properties of SrCu2O2 films deposited on sapphire substrates by pulsed laser deposition

We deposited SrCu₂O₂ (SCO) films on sapphire (Al₂O₃) (0 0 0 1) substrates by pulsed laser deposition. The crystallographic orientation of the SCO thin film showed clear dependence on the growth temperature. X-ray diffraction (XRD) and transmission electron microscopy (TEM) analysis showed that the film deposited at 400 °C was mainly oriented in the SCO [2 0 0] direction, whereas when the growth temperature was increased to 600 °C, the SCO film showed a dominant orientation of SCO [1 1 2]. The SCO film deposited at 500 °C was obvious polycrystalline, showing multi peaks from (2 0 0), (1 1 2), and (2 1 1) diffraction in the XRD spectrum. The SCO film deposited at 600 °C showed a band gap energy of 3.3 eV and transparency up to 80% around 500 nm. The photoluminescence (PL) spectra of the SCO films grown at 500 °C and 600 °C mainly showed blue-green emission, which was attributed to the intra-band transition of the isolated Cu⁺ and Cu⁺–Cu⁺ pairs according to the temperature dependent-PL analysis.     

Optical study of Sr2SnO4:Eu phosphor

This work presents the influence of europium dopant on optical properties of Sr₂SnO₄:Eu³⁺ powders fabricated by a facile low temperature method. Powders were obtained from the same amounts of Eu³⁺ doping into the different concentrations of Sr(NO₃)₂. Powders were examined by means of scanning electron microscopy (SEM), X-ray diffraction (XRD), and photoluminescence (PL). SEM measurements different Eu concentrations in fabricated powders was determined to found different morphologies. XRD analysis revealed the existence of crystalline Sr₂SnO₄ in the form of tetragonal and the diffraction intensity was remarkably changed. PL studies showed a red luminescence of Sr₂SnO₄:Eu³⁺ powders. The intensity of luminescence increased with better crystallinity. This approach provides economically viable route for large-scale synthesis of this kind of nanopowders.     

Surface study of fine MgFe2O4 ferrite powder prepared by chemical methods

To study surface behaviors, MgFe₂O₄ ferrite materials having different grain sizes were synthesized by two different chemical methods, i.e., a polymerization method and a reverse coprecipitation method. The single phase of the cubic MgFe₂O₄ was confirmed by the X-ray diffraction method for both the precursors decomposed at 600-1000 °C except for a very small peak of Fe₂O₃ was detected for the samples calcined at 600 and 700 °C by the polymerization method. The crystal size and particle size increased with an increase in the sintering temperature using both methods. The conductance of the MgFe₂O₄ decreased when the atmosphere was changed from ambient air to air containing 10.0 ppm NO₂. The conductance change, C = G(air)/G(10 ppm NO₂), was reduced with an increase in the operating temperature. For the polymerization method, the maximum C-value was ca. 40 at 300 °C for the samples sintered at 900 °C. However, the samples sintered at 1000 °C showed a low conductance change in the 10 ppm NO₂ gas, because the ratio of the O₂ gas adsorption sites on the particle surface is smaller than those of the samples having a high C-value. The low Mg content on the surface affects the low ratio of the gas adsorption sites. For the reverse coprecipitation method, the particle size was smaller than that of the polymerization method. Although a stable conductance was obtained for the sample sintered at 900 and 1000 °C, its conductance change was less than that of the polymerization method.     

Effects of forming gas annealing on LiNbO3 single crystals

Z-cut congruent LiNbO₃ single crystals were annealed in 95%N₂+5%H₂ at high temperatures. X-ray diffraction showed that 2θ of (0 0 0 6) peak is obviously reduced by 0.6° and 1.0° for the samples annealed at 600 and 900 °C, respectively. A new peak appears at the high-energy side of O 1s spectrum in X-ray photoelelectron spectroscopy (XPS) analyses, and the leakage current is greatly increased. It is proposed that hydrogen is incorporated in LiNbO₃ single crystals through forming gas annealing at temperatures up to 900 °C and exists in LiNbO₃ as a proton bound to an oxygen ion through O-H bond with its electron donated.