Facile Synthesis of Anatase TiO<Subscript>2</Subscript> Nanospheres as Anode Materials for Sodium-Ion Batteries

Anatase TiO₂ nanospheres (ATNSs) were successfully prepared through a facile solvothermal method followed by a thermal treatment. The sample was characterized by scanning electrons microscopy, transmission electron microscopy, x-ray diffraction, Raman spectrum and nitrogen adsorption techniques. When tested as an anode material for sodium-ion batteries, the electrode of ATNSs delivered a large discharge capacity of 208 mAh g^?1 after 100 cycles at a current density of 50 mA g^?1, indicating excellent cycling performance. This could be attributed to the uniform structure of the nanospheres with large surface area and porous nature, providing more active sites, buffering volume change, and facilitating the sodium ion intercalation as well as rapid diffusion during the charge/discharge process. Cyclic voltammetry demonstrated that the sodium storage mechanism is mainly controlled by pseudocapacitive behavior, resulting in a large capacity and outstanding cycling stability.     

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.     

LiMn<Subscript>2</Subscript>O<Subscript>4</Subscript> nanoparticles as cathode in aqueous lithium-ion battery

The aqueous lithium–ion batteries using LiMn₂O₄ as cathode materials are considered to be one of the most promising stationary power sources for large-scale energy storage devices. In the present work, LiMn₂O₄ nanoparticles were successfully synthesized by using sol-gel method, and the morphology of particles was characterized by SEM. We made three electrodes of this active material with PVDF binder and different conductive agents and another electrode of this active material with PTFE binder and Vulcan as a conductor. Electrochemical performances were tested in 5 M LiNO₃ aqueous electrolyte, and comparisons between these electrodes were accomplished.     

Up-Date of a Thermodynamic Database of the ZrO<Subscript>2</Subscript>-Gd<Subscript>2</Subscript>O<Subscript>3</Subscript>-Y<Subscript>2</Subscript>O<Subscript>3</Subscript>-Al<Subscript>2</Subscript>O<Subscript>3</Subscript> System for TBC Applications

The thermodynamic database of the ZrO₂-Gd₂O₃-Y₂O₃-Al₂O₃ system is up-dated taking into account new data on lattice stabilities of ZrO₂, Gd₂O₃ and Y₂O₃ and heat capacity measurements for the monoclinic phase Gd₄Al₂O₉ and phase with garnet structure Gd₃Al₅O₁₂. New data for the heat capacities of Gd₂Zr₂O₇ (pyrochlore) and GdAlO₃ (perovskite) as well as on the enthalpy of formation of fluorite solid solutions (Zr_1−x Gd _x )O_2−x/2 were found to be in good agreement with calculated results. In comparison with the previous assessment, taking into account new experimental data resulted in a change of the melting character of the Gd₄Al₂O₉ phase from a peritectic one to a congruent one in the Gd₂O₃-Al₂O₃ system. Correspondently, in the ternary system ZrO₂-Gd₂O₃-Al₂O₃, the melting character of the three-phase assemblage Gd₂O₃ (B), Gd₄Al₂O₉ and GdAlO₃ changed from eutectic to transition type U. The T ₀-lines for T/M and F/T diffusionless transformations and driving force of partitioning to equilibrium assemblage T + F were calculated in the ZrO₂-Gd₂O₃-Y₂O₃ system.     

Synthesis and electrochemical performance of YF<Subscript>3</Subscript>-coated LiMn<Subscript>2</Subscript>O<Subscript>4</Subscript> cathode materials for Li-ion batteries

Spinel LiMn₂O₄ cathodes were coated with 1 mol% YF₃. X-ray diffraction (XRD) analyses showed that Y and/or F did not enter the lattice of the LiMn₂O₄ crystal. Transmission electron microscopy (TEM) showed that a compact YF₃ layer of 5–20 nm in thickness was coated onto the surface of LiMn₂O₄ particles. Scanning electron microscopy (SEM) observation showed that the YF₃ coating caused the agglomeration of LiMn₂O₄ particles. The cycling test demonstrated that the YF₃ coating can improve the electrochemical performance of LiMn₂O₄ at both 20 and 55°C. Moreover, YF₃-coated LiMn₂O₄ exhibited an improved rate capability compared with the uncoated one at high rates over 5C. The immersion test in electrolytes showed that YF₃-coated LiMn₂O₄ is more erosion resistant than the uncoated one.     

Synthesis and thermal expansion of 4J36/ZrW<Subscript>2</Subscript>O<Subscript>8</Subscript> composites

Gas atomized 4J36 alloy powder was milled for 72 h then mixed with ZrW₂O₈ powder and sintered at 600°C for 4 h under argon atmosphere. 4J36/ZrW₂O₈ composites containing 10 vol.%, 20 vol.%, 30 vol.%, and 40 vol.% ZrW₂O₈ were fabricated, the relative density of which ranged from 70% to 80%. Thermal expansion coefficients of the composites decreased as the amount of ZrW₂O₈ increased, in agreement with the rule of the mixture. The coefficient of thermal expansion of the 4J36/40 vol.%ZrW₂O₈ composite in 25–100°C is 0.55 × 10⁻⁶/°C.     

Floral Biosynthesis of Mn<Subscript>3</Subscript>O<Subscript>4</Subscript> and Fe<Subscript>2</Subscript>O<Subscript>3</Subscript> Nanoparticles Using <Emphasis Type="Italic">Chaenomeles</Emphasis> sp. Flower Extracts for Efficient Medicinal Applications

Manganese oxide (Mn₃O₄) and iron oxide (Fe₂O₃) nanoparticles were successfully synthesized with the flower extracts of Chaenomeles sp. This is the first ever approach to synthesize nanoparticles from Chaenomeles sp. flower extracts. The organic molecules present in the flower extracts actively converted the nitrate precursor into its corresponding nanoparticles. The organic molecules that are involved in the synthesis of nanoparticles are identified using different phytochemical and gas chromatography–mass spectrometry analyses. The identified components are glycosides, alkaloids, terpenoids, saponins, flavonoids, quinines, and steroids. The structural and chemical compositions of the synthesized powder were also analyzed. The x-ray powder diffraction analysis revealed that the particles show tetragonal and rhombohedral crystalline phases. The Fourier transform infrared spectroscopy analysis showed the functional groups that are involved in the reduction of nitrates into the corresponding nanoparticles. Energy-dispersive x-ray spectroscopy analysis confirmed the presence of the elements in the synthesized nanoparticles. Transmission electron microscopy images showed the formation of spherical nanoparticles with an average size of 30–100 nm. Antioxidant analysis showed that the synthesized nanoparticles had excellent antioxidant potential. The antibacterial study showed that they inhibit the growth of harmful bacteria such as Pseudomonas aeruginosa and Streptococcus pyogenes. Thus, this study proposes a new eco-friendly and nontoxic method to synthesize nanoparticles for medicinal applications.     

NiFe<Subscript>2</Subscript>O<Subscript>4</Subscript>-based cermet inert anodes for aluminum electrolysis

Recent developments in the preparation, sintering process, mechanical properties, and thermal shock resistance of cermet inert anodes for aluminum electrolysis are reviewed in this paper. To obtain the desired technologies of low-temperature activated sintering of cermet inert anodes, the effects of material composition, sintering atmosphere, sintering temperature, and sintering aids on the densifi cation and microstructure of NiFe₂O₄-10NiO- based ceramics and cermets were studied. To obtain the toughening and strengthening technology of the cermet, the effects of material composition including ceramic and metallic phases are discussed. The cermet inert anodes with high density and mechanical properties were prepared through adjustment of material composition and sintering technology and selection of feasible sintering aids.     

Fabrication by Electrophoretic Deposition of Nano-Fe<Subscript>3</Subscript>O<Subscript>4</Subscript> and Fe<Subscript>3</Subscript>O<Subscript>4</Subscript>@SiO<Subscript>2</Subscript> 3D Structure on Carbon Fibers as Supercapacitor Materials

Core–shell nanostructured magnetic Fe₃O₄@SiO₂ with particle size ranging from 3 nm to 40 nm has been synthesized via a facile precipitation method. Tetraethyl orthosilicate was employed as surfactant to prepare core–shell structures from Fe₃O₄ nanoparticles synthesized from pomegranate peel extract using a green method. X-ray diffraction analysis, Fourier-transform infrared and ultraviolet–visible (UV–Vis) spectroscopies, transmission electron microscopy, and scanning electron microscopy with energy-dispersive spectroscopy were employed to characterize the samples. The prepared Fe₃O₄ nanoparticles were approximately 12 nm in size, and the thickness of the SiO₂ shell was?~?4 nm. Evaluation of the magnetic properties indicated lower saturation magnetization for Fe₃O₄@SiO₂ powder (~?11.26 emu/g) compared with Fe₃O₄ powder (~?13.30 emu/g), supporting successful wrapping of the Fe₃O₄ nanoparticles by SiO₂. As-prepared powders were deposited on carbon fibers (CFs) using electrophoretic deposition and their electrochemical behavior investigated. The rectangular-shaped cyclic voltagrams of Fe₃O₄@CF and Fe₃O₄@C@CF samples indicated electrochemical double-layer capacitor (EDLC) behavior. The higher specific capacitance of 477 F/g for Fe₃O₄@C@CF (at scan rate of 0.05 V/s in the potential range of ??1.13 to 0.45 V) compared with 205 F/g for Fe₃O₄@CF (at the same scan rate in the potential range of?~???1.04 to 0.24 V) makes the former a superior candidate for use in energy storage applications.     

Synthesis and photocatalytic properties of lanthanum doped anatase TiO<Subscript>2</Subscript> coated Fe<Subscript>3</Subscript>O<Subscript>4</Subscript> composites

A composite photocatalyst (La/TiO<,2>/Fe<,3>O<,4>) with a lanthanum doped TiO<,2> (La/TiO<,2>) shell and a magnetite core was prepared by coating photoactive LafTiO<,2> onto a magnetic Fe<,3>O<,4> core. The morphological, structural, and optical properties of as-prepared samples were charac- terized by transmission electron microscopy (TEM), X-ray diffraction (XRD) and UV-vis absorption spectroscopy. The effect of lanthanum content on the photocatalytie properties was studied, and the result revealed that 0.15 mol% La/TiO<,2>/Fe<,3>O<,4>exhibited the highest photoactiv- ity. The photocatalytic properties of the prepared photocatalyst under UV and visible light were investigated in aqueous solution using methyl orange (MO) as a target pollutant. The results showed that the prepared photocatalyst was activated by visible light and used as an ef- fective catalyst in photooxidation reactions. In addition, the possibility of cyclic usage of the prepared photocatalyst was also confirmed. Moreover, La/TiO<,2> was tightly bound to Fe<,3>O<,4> and could be easily recovered from the medium by a simple magnetic process.     

Experimental study of the Bi<Subscript>2</Subscript>O<Subscript>3</Subscript>-Fe<Subscript>2</Subscript>O<Subscript>3</Subscript> pseudo-binary system

As part of a general contribution to the study of accelerator driven system (ADS) nuclear reactor feasibility, a study of the five-component system Bi-Fe-Hg-O-Pb was undertaken. New results about the quasi-binary Bi₂O₃-Fe₂O₃ are presented in this paper. The phase diagram was reinvestigated by differential scanning calorimetry, x-ray diffraction, and electron probe microanalysis. A new compound was discovered and characterized: Bi₂₅FeO₄₀. Its crystallographic structure was refined. Invariant and transition temperatures are given, as well as phase compositions.     

Fabrication and magnetic properties of NiFe<Subscript>2</Subscript>O<Subscript>4</Subscript> nanorods

NiFe₂O₄ nanorods have been successfully synthesized via thermal treatment of the rod-like precursor fabricated by Ni-doped α-FeOOH, which was enwrapped by the complex of citric acid and Ni²⁺. The morphology evolution during the calcination of the precursor nanorods was investigated with transmission electron microscopy (TEM), and the phase and the magnetic properties of samples were analyzed through X-ray diffraction (XRD) and vibrating sample magnetometer (VSM). The results indicated that the diameter of the NiFe₂O₄ nanorods obtained ranged between 30 and 50 nm, and the length ranged between 2 and 3 μm. As the calcination temperature was up to 600°C, the coercivity, saturation magnetization, and remanent magnetization of the samples were 36.1 kA·m⁻¹, 27.2 A·m²·kg⁻¹, and 5.3 A·m²·kg⁻¹, respectively. The NiFe₂O₄ nanorods prepared have higher shape anisotropy and superior magnetic properties than those with irregular shapes.     

钇掺杂LiFePO4锂离子电池正极材料的制备与性能

用固相法合成LiFe1-xYxPO4 (x=0, 0.01, 0.02, 0.03, 0.04)锂离子电池正极材料,采用X射线衍射仪、扫描电子显微镜、粉末比电阻法和充放电性能测试表征材料的晶体结构、微观形貌、电子电导率和电化学性能。结果表明,少量的钇掺杂并未改变材料的晶体结构,但改善了材料的微观结构,提高其电子电导率,改善可逆容量和电化学性能。在10 mA/g的电流密度下,LiFe0.97Y0.03PO4首次放电容量可达146.54 mAh/g。     

Synthesis of Co_3O_4 Nanoparticles Wrapped Within Full Carbon Matrix as an Anode Material for Lithium Ion Batteries

A facile polyol-assisted pyro-synthesis method was used to synthesize Co_3O_4 nanoparticles embedded into carbon matrix without using any conventional carbon source. The surface analysis by scanning electron microscopy showed that the Co_3O_4 nanoparticles(~20 ± 5 nm) are tightly enwrapped within the carbon matrix. CHN analysis determined the carbon content was only 0.11% in the final annealed sample. The Co_3O_4@carbon exhibited high capacities and excellent cycling performance as an anode at various current rates(such as 914.4 and 515.5 mAh g~(-1) at 0.25 and1.0 C, respectively, after 50 cycles; 318.2 mAh g~(-1) at a high current rate of 5.0 C after 25 cycles). This superior electrochemical performance of the electrode can be attributed to the various aspects, such as,(1) the existence of carbon matrix, which acts as a flexible buffer to accommodate the volume changes during Li~+ion insertion/deinsertion and facilitates the fast Li~+and electron transfer and(2) the anchoring of Co_3O_4 nanoparticles within the carbon matrix prevents particles agglomeration.     

Suspension Plasma-Sprayed ZnFe<Subscript>2</Subscript>O<Subscript>4</Subscript> Nanostructured Coatings for ppm-Level Acetone Detection

Zinc ferrite (ZnFe₂O₄) sensitive coatings have been deposited by suspension plasma spraying. The phase constitution of the coatings was characterized by x-ray diffraction while the top surface and cross-sectional morphology of the coatings were inspected by scanning electron microscopy. The response to acetone was tested with the concentration in the range of 25-500 ppm at the working temperature from 175 to 275 °C. The sensors that were deposited at an arc current of 400 A showed better performance than those at 600 A owing to small grain size and high porosity. The sensor response increased with acetone concentration. The optimized sensors showed excellent response/recovery time and selectivity to acetone at 200 °C.     

Synthesis and Caracterization of Mesoporous FePO<Subscript>4</Subscript> as Positive Electrode Materials for Lithium Batteries

Mesoporous iron phosphates were synthesized using sodium dodecyl sulfate (SDS) and cetyltrimethylammonium bromide (CTAB) as surfactants. The material synthesized in the presence of SDS was not applied as a positive electrode active material of a lithium battery. The results show that the obtained FePO₄ has a mesoporous structure with a specific surface area of 70 m² g^?1 and a dominant pore diameter of 3 nm. Those mesoporous were characterized by different microstructural and electrochemical analyzes. Among the materials studied under different conditions, those calcined at 450°C preserve mesoporous structures and exhibit the best electrochemical performance when used as active materials of the positive electrodes of lithium batteries. Effectively, a relatively high specific capacity of 135 and 122 mAh g^?1 was registered at C/20 collected experimentally by the samples synthesized in the presence of SDS and CTAB, respectively.     

Tunneling magnetoresistance in sintered Fe<Subscript>3</Subscript>O<Subscript>4</Subscript> samples diluted with Fe and α-Fe<Subscript>2</Subscript>O<Subscript>3</Subscript>

Electric transport and magnetoresistance characteristics were investigated for Fe₃O₄-x Fe(x=0, 10, 20 wt.%) samples and Fe₃O₄-α-Fe₂O₃ samples sintered at 500°C. For composition dependence of Fe₃O₄-x Fe samples, the largest room temperature MR, 3.3% at 10 kOe, was obtained from a Fe₃O₄-10 Fe sample. For the surface heat treatment dependence of Fe₃O₄ powders, the largest room temperature MR, 4% at 10 kOe, was obtained from a Fe₃O₄-α-Fe₂O₃ sample sintered with Fe₃O₄ powders heated at 200°C in air. It was found that these enhanced MR ratios always appear together with the appropriate excess resistance which is regarded as the tunneling barrier. These enhanced MR ratios of Fe₃O₄-10 Fe and Fe₃O₄-α-Fe₂O₃ samples can be explained by the increased interparticle contact sites and the appropriate thickness of α-Fe₂O₃, respectively.     

Development and Application of Binary Suspensions in the Ternary System Cr<Subscript>2</Subscript>O<Subscript>3</Subscript>-TiO<Subscript>2</Subscript>-Al<Subscript>2</Subscript>O<Subscript>3</Subscript> for S-HVOF Spraying

Compositions in the system Cr₂O₃-TiO₂-Al₂O₃ are among the most used ceramic materials for thermally sprayed coating solutions. Cr₂O₃ coatings present good sliding wear resistance; Al₂O₃ coatings show excellent insulation behavior and TiO₂ striking corrosion properties. In order to combine these properties, coatings containing more than one oxide are highly interesting. The conventional spraying process is limited to the availability of binary feedstock powders with defined compositions. The use of suspensions offers the opportunity for tailor-made chemical compositions: within the triangle of Cr₂O₃-TiO₂-Al₂O₃, each mixture of oxides can be created. Criteria for the selection of raw materials as well as the relevant aspects for the development of binary suspensions in the Cr₂O₃-TiO₂-Al₂O₃ system to be used as feedstock for thermal spraying are presented. This formulation of binary suspensions required the development of water-based single-oxide suspensions with suitable behavior; otherwise, the interaction between the particles while mixing could lead up to a formation of agglomerates, which affect both the stability of the spray process and the coating properties. For the validation of this formulation procedure, binary Cr₂O₃-TiO₂ and Al₂O₃-TiO₂ suspensions were developed and sprayed using the S-HVOF process. The binary coatings were characterized and discussed in terms of microstructure and microhardness.     

Studies on Al<Subscript>2</Subscript>O<Subscript>3</Subscript>/ZrO<Subscript>2</Subscript>/Al<Subscript>2</Subscript>O<Subscript>3</Subscript> high K gate dielectrics applied in a fully depleted SOI MOSFET

Al₂O₃/ZrO₂/Al₂O₃ gate stacks were prepared on ultrathin SOI (Silicon on insulator) substrates by ultrahigh vacuum electron beam evaporation and post-annealed in N₂ at 450°C for 30 min. Three clear nanolaminate layered structure of Al₂O₃(2.1 nm)/ZrO₂(3.5 nm)/Al₂O₃(2.3 nm) was observed with a high-resolution cross-sectional transmission electron microscope (HR-XTEM). High frequency capacitance voltage (C-V) characteristics of a fully depleted (FD) SOI MOS capacitor at 1 and 5 MHz were studied. The minority carriers determine the high frequency C-V properties, which is opposite to the case of bulk MOS capacitors. The series resistance of the SOI substrate is found to be the determinant factor of the high frequency characteristics of FD SOI MOS capacitors. This article is based on a presentation in “The 7th Korea-China Workshop on Advanced Materials” organized by the Korea-China Advanced Materials Cooperation Center and the China-Korea Advanced Materials Cooperation Center, held at Ramada Plaza Jeju Hotel, Jeju Island, Korea on August 24≈27, 2003.