Controllable synthesis, characterization, and magnetic properties of nanoscale zerovalent iron with specific high Brunauer–Emmett–Teller surface area

This article reports a novel approach for the controllable synthesis of nanoscale zerovalent iron (NZVI) particles with specific high Brunauer–Emmett–Teller (BET) surface areas. Borohydride reduction is a primary and effective liquid phase reduction method for the synthesis of zerovalent iron nanoparticles. However, previous methods for synthesizing NZVI did not suggest a standard technique for controlling the size of particles during the synthesis process; in addition, previous literature generally reported that NZVI had a BET surface area of <37 m²/g. In this communication, a novel approach for the controllable synthesis of NZVI particles with specific high BET surface areas is presented. As a result, the BET surface areas of the NZVI particles synthesized increased to 47.49 and 62.48 m²/g, and the particle sizes decreased to 5–40 and 3–30 nm. Additionally, the physical and chemical properties of the synthesized NZVI particles were investigated by a series of characterizations, and magnetic analysis indicated that the synthesized NZVI particles had super-paramagnetic properties.     

Characterization of the electrical properties of Y2O3-doped CeO2-rich CeO2–ZrO2 solid solutions

Electrical properties of Y₂O₃-doped CeO₂-rich ZrO₂–CeO₂ system were characterized with a view point of its point-defect structural scheme. Theoretical calculation of partial electronic and ionic conductivity from total conductivity was done to investigate the combined homovalent and aliovalent doping effect on the overall electrolytic property. According to our study, combined homovalent and aliovalent doping can be one of the key solutions to overcome the fatal disadvantage of limited electrolytic stability of doped ceria system by which properly enhances the ionic conductivity and suppresses the electronic conductivity all at once. Feasibility and limitation of Y₂O₃-doped CeO₂-rich ZrO₂–CeO₂ system as a potential alternative electrolyte material for low or intermediate temperature SOFC were discussed.     

Influence of sintering conditions on the electrical properties of 10% ZrO2–10% Y2O3–CeO2 (mol%)

Yttria–zirconia doped ceria, 10% ZrO₂–10% Y₂O₃–CeO₂ (mol%) (CZY) and 0.5 mol% alumina-doped CZY (CZYA), prepared through oxide mixture process, were sintered by isothermal sintering (IS) and two-step sintering (TSS) having as variable the temperature and soaking time. The electrical conductivity of sintered samples was investigated in the 250 to 600 °C temperature range by impedance spectroscopy in air atmosphere. The microstructure was analyzed by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Alumina, as additive, improves the grain boundary conductivity of samples sintered at temperatures lower than 1500 °C. Concerning the sintering mode, two-step sintering (TSS) proved to be a good procedure to obtain CZYA samples with high electrical conductivity and density (> 95%) at relatively low sintering temperature and long soaking time.     

Mechanical Response of ZrB2–SiC–ZrO2 Composite Laminate

Russian Physics Journal - The paper deals with heat-reflecting ZrB2–20% SiC ceramic composite and heat-reflecting ZrB2–20% SiC composite laminate with ZrO2 addition, the amount of which...     

Ceramic synthesis of 0.08BiGaO_3–0.90BaTiO_3–0.02LiNbO_3 under high pressure and high temperature

In this paper, the preparation of 0.08BiGaO_3–0.90BaTiO_3–0.02LiNbO_3 is investigated at pressure 3.8 GPa and temperature 1100–1200?C. Experimental results indicate that not only is the sintered rate more effective, but also the sintered temperature is lower under high pressure and high temperature than those of under normal pressure. It is thought that the adscititious pressure plays the key role in this process, which is discussed in detail. The composition and the structure of the as-prepared samples are recorded by XRD patterns. The result shows that the phases of Ba TiO_3, BaBiO_(2.77), and Ba_2Bi_4Ti_5O_(18) with piezoelectric ceramic performance generate in the sintered samples. Furthermore, the surface morphology characteristics of the typical samples are also investigated using a scanning electron microscope. It indicates that the grain size and surface structure of the samples are closely related to the sintering temperature and sintering time. It is hoped that this study can provide a new train of thought for the preparation of lead-free piezoelectric ceramics with excellent performance.     

Ultrasound and microwave assisted synthesis of high loading Fe-supported Fischer–Tropsch catalysts

Supported iron-based Fischer–Tropsch (FT) catalysts with high loading of active metal have been prepared using both traditional and innovative methods. In these latter the impregnation of silica support has been performed by adding a step involving an ultrasound (US) or a microwave (MW) treatment to improve the metal deposition and to increase the catalyst activity. FT results have indicated the catalysts prepared by US as the most efficient, particularly when sonication is performed in argon atmosphere. MW prepared samples have given results very similar to those obtained with the traditional method. In order to explain the different catalytic activity, all the samples have been characterized by BET, TPR, SEM, TEM, XRD and micro-Raman analyses.     

Fabrication and Characterization of Bioglass-Modified HA–ZrO2 Biocomposites

Hydroxyapatite (HA) being the main mineral constituent of human hard tissues is highly bioactive. Good chemical bonds can be generated between HA and natural bone. However, the low strength and inherent brittleness of HA restrict its application usually to non-load-bearing conditions. In this work, production of a new kind of HA–ZrO₂ composite by hot-press sintering method is described. Bioglass which has been widely used in reconstruction of damaged or diseased tissues was added into HA–ZrO₂ composites. Comparing with pure HA ceramic, this type of composite possesses better mechanical strength and retains the bioactivity of HA as well. The liquid phase generated by bioglass has been effective in improving the sintering process of HA–ZrO₂ composites. The phase composition of HA composite was characterized by XRD and their fracture surfaces were observed by SEM. The XRD results show that introducing a small amount of bioglass into HA–ZrO₂ composite cannot enhance decomposition of HA. The SEM images show that there were fewer pores on the fracture surfaces of HA–ZrO₂–bioglass composite than in the HA–ZrO₂ composite. The flexural strength and toughness of HA–ZrO₂ composite containing 2 wt% bioglass were 157 MPa and 1.63 MPa·m^1/2, respectively.     

Thermophoresis-assisted vapour phase synthesis of CeO2 and CexY1−xO2−δ nanoparticles

Thermophoresis-assisted chemical vapour deposition (CVD) was used to produce nano-sized particles of ceria and yttria-doped ceria. The solid precursors cerium trichloride and yttrium trichloride were used with oxygen. After homogeneous nucleation, condensation and coagulation, thermophoresis-assisted particle collection was achieved in two different ways. Particle dimensions were studied by transmission electron microscopy (TEM) and X-ray diffraction (XRD)-line broadening. Crystallite and particle dimensions varied from 9 to 30 nm and from 30 to 80 nm, respectively. The influence of process conditions is discussed.     

Preparation of CeO2 by a simple microwave–hydrothermal method

Cerium carbonate hydroxide (orthorhombic Ce(OH)CO₃) hexagonal-shaped microplates were synthesized by a simple and fast microwave–hydrothermal method at 150 °C for 30 min. Cerium nitrate, urea and cetyltrimethylammonium bromide were used as precursors. Ceria (cubic CeO₂) rhombus-shape was obtained by a thermal decomposition oxidation process at 500 °C for 1 h using as- synthesized Ce(OH)CO₃. The products were characterized by X-ray powder diffraction, field-emission scanning electron microscopy, thermogravimetric analysis and Fourier transformed infrared spectroscopy. The use of microwave–hydrothermal method allowed to obtain cerium compounds at low temperature and shorter time compared to other synthesis methods.     

Specific Features of the Local Structure and Transport Properties of ZrO2–Sc2O3–Y2O3 and ZrO2–Sc2O3–Yb2O3 Crystals

Optics and Spectroscopy - The specific features of the local structure of ZrO2–Sc2O3–Y2O3 and ZrO2–Sc2O3–Yb2O3 crystals are revealed by optical spectroscopy using the Eu3+...     

Optical Properties of ZrO2–Containing Anodic Coatings on Aluminum

Anodic oxide coatings (AOC) formed at the potentials of spark breakdowns in aqueous solutions of potassium hexafluorozirconate (K₂ZrF₆) contain up to 36 wt.% of Zr. The modification of ZrO₂ in AOC is tetragonal. The reflection coefficients of AOC have been measured in the range 430–670 nm. After UV irradiation for a few hours the reflection coefficient decreases by several percent. The treatment of AOC in a solution containing F^– and [Fe(CN)]^3– ions leads to a change in the aluminum and zirconium concentrations in the surface layer and to an increase of the AOC reflectivity.     

Comparative study of aerogels nanostructured catalysts: Ni/ZrO2–SO4 2− and Ni/ZrO2–Al2O3–SO4 2−

Ionics - A series of Ni/ZrO2–SO4 2− and Ni/ZrO2–Al2O3–SO4 2− catalysts were prepared in one step by the sol–gel method and dried in hypercritical conditions of...     

Solid-phase synthesis of manganese silicides on the Si(100)2 × 1 surface

The solid-phase synthesis of manganese silicides on the Si(100)2 × 1 surface coated at room temperature by a 2-nm-thick manganese film has been investigated using high-energy-resolution photoelectron spectroscopy with synchrotron radiation. The dynamics of variation of the phase composition and electronic structure of the near-surface region with increasing sample annealing temperature to 600°C, has been revealed. It has been shown that, under these conditions, a solid solution of silicon in manganese, metallic manganese monosilicide MnSi, and semiconductor silicide MnSi_1.7 are successively formed on the silicon surface. The films of both silicides are not continuous, with the fraction of the substrate surface occupied by them decreasing with increasing annealing temperature. The binding energies of the Si 2p and Mn 3p electrons in the compounds synthesized have been determined.     

Improvement of Cu–CeO2 anodes for SOFCs running on ethanol fuels

Ethanol is considered to be an attractive green fuel for solid oxide fuel cells (SOFCs) due to several advantages. In this paper, we presented recent progress of our group in Cu–CeO₂ anodes for SOFCs with ethanol steam as a fuel. Cu–CeO₂–ScSZ (scandia stabilized zirconia)anodes with different ratios of copper versus ceria were fabricated and the impedance spectra of symmetric cells were measured to optimize the anode composition. Area specific resistance (ASR) of these anodes was examined to prove the thermal stability of them, and possible reasons for degradation were analyzed. Furthermore, a Ni–ScSZ interlayer was added between Cu–CeO₂–YSZ (yttria stabilized zirconia) anode and ScSZ electrolyte to improve the anode performance, and the three-layer structure was fabricated by acid leaching of nickel and wet impregnation method. The maximum power density of the single cell reached 604 mW cm^? 2 and 408 mW cm^? 2 at 800 °C in hydrogen and ethanol steam respectively, and the cell obtained stable output in ethanol steam over an operation period of 50 h.     

Simple synthesis of ironIII sulfophenyl phosphate nanosheets as a high temperature inorganic–organic proton conductor

Iron^III sulfophenyl phosphate (FeSPP) is successfully synthesized by an optimized process from the reaction of iron^III chloride and m-sulfophenyl phosphonic acid (msPPA) by a simple and environmentally friendly method. Experimental results show FeSPP has a kind of layered structure, and multilayer sheet is about 2 nm thick. FeSPP exhibits good thermal stability and does not decompose under 200 °C. Protons transfer through vehicle and Grotthuss mechanisms at different relative humidities (RH). The conductivity of FeSPP can reach to 0.115 S/cm at 180 °C and RH?=?100 %. Under this condition, vehicle mechanism plays the leading role, and the Grotthuss mechanism plays the minor role. At low RH, Grotthuss plays the leading role, and vehicle plays the minor role. In a drying oven at 180 °C, the proton conductivity remains 2.15?×?10^?3 S/cm. Good conductivities at different RH and thermal stabilities clearly demonstrate that FeSPP is a highly effective conductor. It can be used as catalysts, chemical sensors, and in the preparation of composite membrane.     

Effect of TiO2 addition on the crystallization of quenched glasses in the SiO2–Al2O3–ZrO2 system

The glass formation in the SiO₂-rich region of the ternary oxide system Al₂O₃–ZrO₂–SiO₂ with MgO, CaO, and TiO₂ as melting aids was analyzed. The crystallization of glasses with different content of TiO₂ and phase evolution with the temperature was studied by X-ray diffraction, infrared, laser Raman spectroscopy and transmission electron microscopy. The use of TiO₂ favored formation and crystallization of the glasses due to the decrease of the viscosity of melts and acting as a nucleating agent. The crystalline phase of t-ZrO₂ was developed at temperatures as low as 880°C whereas in as prepared specimens without TiO₂ its presence was not detected. For the specimens with TiO₂, t-ZrO₂ and mullite were the principal phases at 1000°C. TiO₂ addition did not change the crystallization sequence but decreased the formation temperature of the crystalline phases. Most of Ti⁴⁺ ions entered into t-ZrO₂ and only a small portion in mullite, but the surplus was detected in ZrTiO₄.     

Structural evolution of ZrO2–mullite nanocomposites from the Si–Al–Zr–O amorphous bulk

ZrO₂–mullite nanocomposites were fabricated by in-situ-controlled crystallization of Si–Al–Zr–O amorphous bulk at 800–1250°C. The structural evolution of the Si–Al–Zr–O amorphous, annealed at different temperatures, was studied by X-ray diffraction, infrared, Laser Raman spectroscopy, field emission scanning electron microscopy, and high-resolution transmission electron microscopy. The materials consisted of an amorphous phase up to 920°C at which phase separation of Si-rich and Al, Zr-rich clusters occurred. The crystalline phases of t-ZrO₂ and mullite were observed at 950°C and 1000°C, respectively. Mullite with a tetragonal structure, formed by the reaction between Al–Si spinel and amorphous silica at low temperature, changed into an orthorhombic structure with the increase of temperature. It was the phase segregation that improved crystallization of the Si–Al–Zr–O amorphous bulk. The anisotropic growth of mullite was observed and the phase transformation from t-ZrO₂ to m-ZrO₂ occurred when the temperature was higher than 1100°C.     

Ultrasonic,FTIR and thermal investigations of SiO2–Na2O–CaO–P2O5 glasses doped with CeO2

The longitudinal and shear ultrasonic wave velocities for different compositions of SiO₂–Na₂O–CaO–P₂O₅ glasses were measured at room temperature (305 K) using a pulse-echo method at a frequency of 4 MHz. The elastic moduli, Poisson's ratio, microhardness, Debye temperature and other ultrasonic parameters were obtained from experimental data and analyzed using bond compression theory. By calculating the number of network bonds per unit volume, the average stretching constant, and the average ring size, information about the structure of the glass can be deduced. Structural changes after doping with CeO₂ were investigated by FTIR spectroscopy, and by measurements of the thermal expansion coefficient, glass transition and softening temperature to throw more light on the characterization of these glasses.