Controllable Low-Temperature Hydrothermal Synthesis and Gas-Sensing Investigation of Crystalline SnO<Subscript>2</Subscript> Nanoparticles

SnO₂ nanoparticles have been successfully synthesized by a facile hydrothermal method from SnCl₂·2H₂O, hexamethylenetetramine, and trisodium citrate in water at 120 °C for 12 h. The effects of surfactant and precipitant on SnO₂ synthesis were investigated. SnO₂ nanoparticles can be synthesized in the temperature range of 120-180 °C with long reaction time in the presence of trisodium citrate. When NaOH was used as precipitant instead of hexamethylenetetramine, it is difficult to obtain SnO₂ nanoparticles at 120 °C in the presence of trisodium citrate. SnO₂ nanoparticles with an average size of about 5 nm show good crystallinity and excellent sensitivity to ethanol and acetaldehyde in about 55% relative humidity.     

Synthetically Controlled,Carbon-Coated Co<Subscript>2</Subscript>SnO<Subscript>4</Subscript>/SnO<Subscript>2</Subscript> Composite Anode for Lithium-ion Batteries

The inherent drawbacks of Co₂SnO₄ in demonstrating the closer-to-theoretical capacity value behavior and the inadmissible volume-expansion-related capacity fade behavior have been surpassed by choosing a tailor-made material composition of Co₂SnO₄/SnO₂, prepared at two different temperatures such as 400°C and 600°C to obtain residual carbon-containing and carbon-free compositions, respectively. Among the products, carbon-coated Co₂SnO₄/SnO₂ composite exhibits better electrochemical performance compared with that of the carbon-free product mainly because of the beneficial effect of carbon in accommodating the volume-expansion-related issues arising from the alloying/de-alloying mechanism. A combination of conversion reaction and alloying/de-alloying mechanism is found to play a vital role in exhibiting closer-to-theoretical capacity values. In other words, an appreciable specific capacity value of 834 mAh g^?1 has been exhibited by Co₂SnO₄/SnO₂ anode containing carbon coating, thus, demonstrating the possibility to improve the electrochemical performance of the title anode through carbon coating, which is realized as a result of the addition of carefully manipulated synthesis conditions.     

Synthesis and electrochemical properties of SnO2-CuO nanocomposite powders

1 Introduction Since YOSHIO et al[1] announced the commercia- lization of tin oxide as negative electrodes of 1ithium-ion batteries, the tin oxide anode has attracted much attention due to its high specific capacity, which is about twice that of graphite…     

Corrosion of Inconel 690 in N<Subscript>2</Subscript>-0.1%H<Subscript>2</Subscript>S gas at 700-800 °C

Inconel 690 superalloy was corroded at 700 °C and 800 °C for up to 70 h in N₂-0.1% H₂S gas. It corroded almost linearly with large weight gains, displaying little protectiveness. Its corrosion rates were quite fast when compared with its corrosion in air or Ar-1%SO₂ gas. The formed scales were thick, fragile, and nonadherent. They consisted primarily of Cr₂O₃ with some NiCr₂O₄, Ni₃S₂, CrS, and Cr₂S₃. The H₂S gas accelerated the corrosion significantly by forming nonprotective sulfides and dissolving hydrogen in the scale and in the internal corrosion zone that consisted of discrete chromium-sulfides and some oxide particles. The marker test indicated that the scales grew by the outward diffusion of metallic ions such as Ni, Cr, Fe, and Mn, whilst the internal corrosion zone thickened by the inward migration of oxygen and sulfur through the lattice, grain boundaries, and microcracks.     

Experimental investigation and thermochemical assessment on the SnO<Subscript>2</Subscript>-CuO system

Differential thermal analysis/theromgravimetry (DTA/TG) measurements performed in air have established that above 1273 K the SnO₂-CuO initially stochiometric system transforms into a system of the SnO₂-CuO_x type, with the value of x depending on temperature T and p _{O 2} oxygen partial pressure values. The dissociation process of CuO to Cu₂O, as well as the formation of a liquid phase with an uptake of oxygen, has been experimentally verified. Above the minimum value of the oxygen partial pressure for which the only components of the system are SnO₂ and CuO (i. e., over p_{O 2} = 24 atm), the phase diagram was calculated by modeling the behavior of the liquid phase with a sub-regular approximation. A homogeneous liquid phase with no tendency toward immiscibility was found to be energetically favorable over the entire compositional range of the SnO₂-CuO system for T ≥ 1470 K. As a result of the calculations, the phase diagram is given for p_{O 2} = 24 atm; the diagram is a simple eutectic type with the eutectic composition placed in the CuO-rich domain (i.e., copper oxide molar fraction x = 0.873 and melting at 1470 K). The phase diagram calculated for the SnO₂-CuO system is compared with the data reported for other CuO-based systems.     

Subsolidus Phase Relations of the CaO-REO<Subscript>x</Subscript><Emphasis Type="Bold">-</Emphasis>CuO Systems (RE = Eu,Tb, Dy,Ho, Er,Lu and Sc) at 900 °C in Air

The subsolidus phase relations of the CaO-REO_x-CuO systems (RE = Eu, Tb, Dy, Ho, Er, Lu and Sc) were investigated in air at 900 °C. The pseudo-ternary sections with RE = Tb, Dy, Ho, Er and Lu have a similar structure. They have in common with the RE = Eu system a solid solution of Ca_0.833?xRE_xCuO_2+y composition but the system with RE = Eu differs by the presence of an Eu₂CuO₄ phase instead of RE₂Cu₂O₅ for RE = Tb, Dy, Ho, Er and Lu. In contrast, the CaO-ScO_1.5-CuO section does not contain a Ca_0.833?xSc_xCuO_2+y solid solution and is dominated by the CaSc₂O₄ phase, which has no equivalent in the other systems at 900 °C in air.     

NO2 gas sensing based on ordered ultrathin films of conducting polymer and its nanocomposite

The metal oxides films are widely used for CO, aromatic hydrocarbon and NO₂, gas-sensing applications, but such sensors mostly lack selectivity and operate at high temperatures (300–500 °C). We focused on the use of organized ultrathin films of conducting polymers and their nanocomposites, which recognize selectively the NO₂ gases with a very high sensitivity (≤ppb). Polyhexylthiophene (PHTh), poly(ethylene dioxythiophene) (PEDT), PHTh–PEDT copolymer, sulfonated polyaniline, polyaniline (PANI)–SnO₂, polypyrrole (PPy)–SnO₂, PEDT-SnO₂, PHTh–SnO₂ and copolymer (HTh-EDT)–SnO₂ conducting polymer and nanocomposite thin films were fabricated and used for gas sensing applications. The physical properties (UV and FTIR) such films were investigated before and after the NO₂ gas treatment. Regioregular PHTh, its copolymer P(HTh-PEDT), and their metal oxide nanocomposites films detected NO₂ gas with a high sensitivity.     

Preparation and magnetic properties of Fe<Subscript>2</Subscript>O<Subscript>3</Subscript> microtubules prepared by sol-gel template method

Fe(OH)₃ precursor sol was prepared by a sol-gel method. The precursor sol was dipped onto the absorbent cotton, and gel was formed on the absorbent cotton template after the volatilization of moisture. Fe₂O₃ microtubules were synthesized after the process of self-propagation or calcination. The phase, morphology, and particle diameter of the samples were examined by X-ray diffraction (XRD) and scanning electron microscopy (SEM), and the magnetic properties of the samples were measured using a vibrating sample magnetometer (VSM). The external diameters of Fe₂O₃ microtubules ranged between 8 and 13 μm, and the wall thicknesses ranged between 0.5 and 2 μm. The type of the calcination method plays a significant role in developing the Fe₂O₃ phase and the variation in the magnetic properties in the sol-gel template complexing method. γ-Fe₂O₃ was synthesized by a self-propagation method. However, α-Fe₂O₃ was synthesized after calcination at 400°C for 2 h. The coercivity of the samples synthesized by calcination at 400°C for 2 h after self-propagation was found to increase significantly, thereby presenting hard magnetic properties.     

Evaluation of in vitro and in vivo tests for surface-modified titanium by H<Subscript>2</Subscript>SO<Subscript>4</Subscript> and H<Subscript>2</Subscript>O<Subscript>2</Subscript> treatment

Titanium is widely used as an implant material for artificial teeth. Furthermore, various studies have examined surface treatment with respect to the formation of a fine passive film on the surface of commercial titanium and its alloys and to improve the bioactivity with bone. However, there is insufficient data about the biocompatibility of implant materials in the body. The purpose of this study was to examine whether surface modification affects the precipitation of apatite on titanium metal. Specimens were chemically washed for 2 min in a 1∶1∶1.5 (vol.%) mixture of 48 %HF, 60%HNO₃ and distilled water. The specimens were then chemically treated with a solution containing 97%H₂SO₄ and 30%H₂O₂ at the ratio of 1∶1 (vol.%) at 40°C for 1h, and subsequently heat-treated at 400°C for 1h. All the specimens were immersed in HBSS with pH 7.4 at 36.5°C for 15d, and the surface was examined with TF-XRD, SEM, EDX and XPS. In addition, specimens of commercial pure Ti, with and without surface treatment, were implanted in the abdominal connective tissue of mice for 28 d. Conventional aluminum and stainless steel 316L were also implanted for comparison. An amorphous titania gel layer was formed on the titanium surface after the titanium specimen was treated with a solution of H₂SO₄ and H₂O₂. The average roughness was 2.175 μm after chemical surface treatment. The amorphous titania was subsequently transformed into anatase by heat treatment at 400°C for 1h. The average thickness of the fibrous capsule surrounding the specimens implanted in the connective tissue was 47.1μm in the chemically treated Ti, and 52.2, 168.7 and 101.9μm, respectively, in the untreated commercial pure Ti, aluminum and stainless steel 316L.     

Al<Subscript>2</Subscript>O<Subscript>3</Subscript>-TiC Composite Prepared by Spark Plasma Sintering Process: Evaluation of Mechanical and Tribological Properties

Al₂O₃-10TiC composites were synthesized by spark plasma sintering (SPS) process. Microstructural and mechanical properties of the composite reveal homogeneous distribution of the fine TiC particles in the matrix. The samples were produced with different sintering temperature, and it shows that the hardness and density gradually increases with increasing sintering temperature. Abrasion wear test result reveals that the composite sintered at 1500 °C shows high abrasion resistance (wt. loss ~ 0.016 g) and the lowest abrasion resistance was observed for the composite sample sintered at 1100 °C (wt. loss ~ 1.459 g). The profilometry surface roughness study shows that sample sintered at 1100 °C shows maximum roughness (R_a = 6.53 µm) compared to the sample sintered at 1500 °C (R_a = 0.66 µm) corroborating the abrasion wear test results.     

Preparation and characterization of nanostructured Bi<Subscript>2</Subscript>Se<Subscript>3</Subscript> and Sn<Subscript>0.5</Subscript>-Bi<Subscript>2</Subscript>Se<Subscript>3</Subscript>

Nanostructured Bi₂Se₃ and Sn_0.5-Bi₂Se₃ were successfully synthesized by hydrothermal coreduction from SnCl₂·H₂O and the oxides of Bi and Se. The products were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), and field emission scanning electron microscope (FESEM). Bi₂Se₃ powders obtained at 180°C and 150°C consist of hexagonal flakes of 50–150 nm in side length and nanorods of 30–100 nm in diameter and more than 1 μm in length. The product obtained at 120°C is composed of thin irregular nanosheets with a size of 100–200 nm and several nanometers in thickness. The major phase of Sn_0.5-Bi₂Se₃ synthesized at 180°C is similar to that of Bi₂Se₃. Sn_0.5-Bi₂Se₃ powders are primarily nanorod structures, but small amount of powders demonstrate irregular morphologies.     

Nanostructural Free-Volume Effects in Humidity-Sensitive MgO-Al<Subscript>2</Subscript>O<Subscript>3</Subscript> Ceramics for Sensor Applications

Technologically modified spinel MgO-Al₂O₃ ceramics were prepared from Al₂O₃ and 4MgCO₃·Mg(OH)₂·5H₂O powders at sintering temperatures of 1200, 1300, and 1400 °C. Free-volume structural effects in MgO-Al₂O₃ ceramics and their electrophysical properties were studied using combined x-ray diffraction, scanning electron microscopy, Hg-porosimetry, and positron annihilation lifetime spectroscopy. It is shown that increasing of sintering temperature from 1200 to 1400 °C results in the transformation of pore size distribution in ceramics from tri- to bi-modal including open macro- and meso(micro)pores with sizes from ten to hundreds nm and nanopores with sizes up to a few nm. Microstructure of these ceramics is improved with the increase of sintering temperature, which results in decreased amount of additional phases located near grain boundaries. These phase extractions serve as specific trapping centers for positrons penetrating the ceramics. The positron trapping and ortho-positronium decaying components are considered in the mathematical treatment of the measured spectra. Classic Tao-Eldrup model is used to draw the correlation between the ortho-positronium lifetime and the size of nanopores, which is complementary to porosimetry data. The studied ceramics with optimal nanoporous structure are highly sensitive to humidity changes in the region of 31-96% with minimal hysteresis in adsorption-desorption cycles.     

The role of Ce ions in electrochemical corrosion of 304 SS in Ce(NO<Subscript>3</Subscript>)<Subscript>3</Subscript>.6H<Subscript>2</Subscript>O

Effects of temperature and potential on the electrochemical corrosion behavior of alloy AISI 304 (UNS S30400) Stainless steel were investigated in 3 wt.% cerium nitrate (Ce[NO₃]₃.6H₂O) solution. With an increase in electrolyte temperature from ambient temperature to 90°C, the corrosion potential of the alloy shifted towards the noble direction, and the resistance to polarization increased due to the formation of Ce-oxide on the electrode surface. The oxide films formed at the open circuit potential (OCP) and a passive potential of 0.4 V_SCE were examined by x-ray photoelectron spectroscopy (XPS). The oxide film formed at 50°C and a passive potentialof 0.4 V_SCE consists of mixed oxides of Ce and Cr, whereas that at OCP consists of only Cr oxide. The formation of Cr oxides on the electrode surface was primarily due to the nitrate (NO₃ ⁻) ions in Ce(NO₃)₃.6H₂O electrolyte.     

Hydrogen generation from the H<Subscript>2</Subscript>O/H<Subscript>2</Subscript>O<Subscript>2</Subscript> /MnMoO<Subscript>4</Subscript> system

Hydrogen gas as a clean energy resource was found to be largely bubbled from the H₂O/H₂O₂/MnMoO₄ system. The MnMoO₄ powder was synthesized by a sol-gel method and was characterized with x-ray diffraction, transmission electron microscopy, and x-ray photoelectron spectrometry. The efficiency of the hydrogen generation increases with increasing H₂O₂ proportion, amount of MnMoO₄ powder, and intensity of light resource. A mechanism is suggested for hydrogen generation from the H₂O/H₂O₂/MnMoO₄ system.     

Effects of H<Subscript>2</Subscript> Atmospheres on Sintering of Low Alloy Steels Containing Oxygen-Sensitive Masteralloys

Processing of novel sintered steels with compositions including oxygen-sensitive elements requires deep understanding of the chemistry of sintering. The use of H₂ atmospheres alleviates the oxygen transference from the base powder to the oxygen-sensitive particles. However, in H₂, methane formation at 700–1200°C causes dramatic homogeneous decarburization of the part that affects both mechanical behavior and dimensional stability. The intensity and the critical temperatures of this effect depend strongly on the alloying elements, being significantly enhanced in presence of Si. When combining the alloying elements as Fe-Mn-Si masteralloys, methane formation is enhanced around 760°C due to the high Mn content (40 wt.%) in the masteralloys. Nevertheless, the benefits of H₂ towards oxide reduction can still be advantageously used if diluting it in the form of N₂-H₂ atmospheres, or if limiting the use of H₂ to temperatures below 500°C. Thus, decarburization due to methane formation can be successfully controlled.     

Preparation and microstructure characterization of a nano-sized Ti<Superscript>4+</Superscript>-doped AgSnO<Subscript>2</Subscript> electrical contact material

A Ti⁴⁺-doped nano-structured AgSnO₂ material was prepared using sol-gel method and characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), and scanning electron microscopy (SEM). The results show that Ti⁴⁺ cations are successfully doped into the crystal lattice of SnO₂, and thus significantly improve the electrical conductivity of the sample. Furthermore, the coating of Ag on Ti⁴⁺-doped SnO₂ nano-sized particles enhances the surface wettability and enables the resulting AgSnO₂ material to have better mechanical properties.     

Electrochemical properties of spinel compound LiNi_（0.5）Mn_（1.2）Ti_（0.3）O_4 as cathode materials for lithium ion batteries

The electrochemical properties of spinel compound LiNi0.5Mn1.2Ti0.3O4 were investigated in this study.The chemicals LiAc·2H2O,Mn(Ac)2·2H2O,Ni(Ac)2·4H2O,and Ti(OCH3)4 were used to synthesize LiNi0.5Mn1.2Ti0.3O4 by a simple sol-gel method.The discharge capacity of the sample reached 134 mAh/g at a current rate of 0.1C.The first and fifth cycle voltammogram almost overlapped,which showed that the prepared sample LiNi0.5Mn1.2Ti0.3O4 had excellent good cycle performance.There were two oxidation peaks at 4.21 V and 4.86 V,and two reduction peaks at 4.55 V and 3.88 V in the cycle voltammogram,respectively.By electrochemical impedance spectroscopy and its fitted result,the lithium ion diffusion coefficient was measured to be approximately 7.76 × 10?11 cm2/s.     

Synthesis,Fabrication and Characterization of ZnO-Based Thin Films Prepared by Sol–Gel Process and H<Subscript>2</Subscript> Gas Sensing Performance

In this paper, an attempt is made to deposit ZnO thin films using sol–gel process followed by dip-coating method on p-silicon (100) substrates for intended application as a hydrogen gas sensor owing to the low toxic nature and thermal stability of ZnO. The thin films are annealed under annealing temperatures of 350, 450 and 550 °C for 25 min. The crystalline quality of the fabricated thin films is then analyzed by field-emission scanning electron microscopy and transmission electron microscope. The gas sensing performance analysis of ZnO thin films is demonstrated at different annealing temperatures and hydrogen gas concentrations ranging from 100 to 3000 ppm. Results obtained show that the sensitivity is significantly improved as annealing temperature increases with maximum sensitivity being achieved at 550 °C annealing temperature and operating temperature of 150 °C. Hence, the modified ZnO thin films can be applicable as H₂ gas sensing device showing to the improved performance in comparison with unmodified thin-film sensor.     

Hydrogen storage properties of as-cast and annealed low-Co La<Subscript>1.8</Subscript>Ti<Subscript>0.2</Subscript>MgNi<Subscript>8.9</Subscript>Co<Subscript>0.1</Subscript> alloys

Low-Co La_1.8Ti_0.2MgNi_8.9Co_0.1 alloys were prepared by magnetic levitation melting followed by annealing treatment. The effect of annealing on the hydrogen storage properties of the alloys was investigated systematically by X-ray diffraction (XRD), pressure-composition isotherm (PCI), and electrochemical measurements. The results show that all samples contain LaNi₅ and LaMg₂Ni₉ phases. LaCo₅ phase appears at 1,000 °C. The enthalpy change of all hydrides is close to ?30.6 kJ·mol^?1 H₂ of LaNi₅ compound. Annealing not only increases hydrogen capacity and improves cycling stability but also decreases plateau pressure at 800 and 900 °C. After annealing, the contraction of cell volume and the increase of hydride stability cause the high rate dischargeability to reduce slightly. The optimum alloy is found to be one annealed at 900 °C, with its hydrogen capacity reaching up to 1.53 wt%, and discharge capacity remaining 225.1 mAh·g^?1 after 140 charge–discharge cycles.     

碳纳米管修饰的空心多孔NiO/SnO2纳米复合材料对丙酮传感性能的优化

通过静电纺丝法制备中空多孔的NiO/SnO2复合纳米纤维,在复合纤维表面装饰碳纳米管,在此基础上制备气敏传感器器件。利用TGA确定了复合材料热分解温度,得到热处理工艺;利用SEM、XRD、TEM、XPS分别对复合材料的形貌、结构、尺寸、表面成分进行了表征。使用WS-30A气敏元件测试仪对气敏元件响应进行测试,结果表明CNTs装饰的NiO/SnO2复合纳米材料制备的气敏传感器降低了丙酮检测最佳工作温度,为160℃,提高了检测灵敏度,对50 ppm丙酮的响应达到25.25,对检测丙酮有快速的响应(~8.2 s)以及恢复性能(~10.5 s),同时在30天的长期稳定性测试中也体现了良好的稳定性。证明了装饰CNTs 的 NiO/SnO₂复合材料在检测丙酮方面的潜在价值,同时本文也进一步讨论了CNTs, 中空多孔结构的NiO/SnO₂提高检测性能的作用机理。