Synthesis and characterization of Fe(III)-silicate precipitation tubes

Fe(III)-silicate precipitation tubes synthesized through “silica garden” route have been characterized using a number of analytical techniques including X-ray diffraction, infrared spectroscopy, atomic force microscopy, scanning and transmission electron microscopy. These tubes are brittle and amorphous and are hierarchically built from smaller tubes of 5-10 nm diameters. They remain amorphous at least up to 650 °C. Crystobalite and hematite are the major phases present in Fe(III)-silicate tubes heated at 850 °C. Morphology and chemical compositions at the external and internal walls of these tubes are remarkably different. These tubes are porous with high BET surface area of 291.2 m²/g. Fe(III)-silicate tubes contain significant amount of physically and chemically bound moisture. They show promise as an adsorbent for Pb(II), Zn(II), and Cr(III) in aqueous medium.     

Growth of crystalline YbVO4 thin-film optical waveguides by pulsed laser deposition

Epitaxial YbVO₄ films have been grown on sapphire and Si/SiO₂ substrates by pulsed laser deposition. Films were grown over a range of temperatures from 600 to 700 °C in the presence of an oxygen pressure between 2 and 20 Pa. The films were characterized by X-ray diffraction (XRD), atomic force microscopy (AFM), high-resolution scanning electron microscopy (HRSEM), and dark-mode prism coupling measurements. YbVO₄ films show epitaxial growth and display one main axis orientation of (2 0 0). The degree of crystal orientation increases with increasing depositing temperature and oxygen pressure up to 700 °C and 20 Pa, respectively. AFM and HRSEM measurements show that the prepared films are dense and homogeneous and three-dimensional-island growth mechanism is confirmed. According to prism coupling measurements, sharp dip is observed for both transverse-electric (TE) and transverse-magnetic (TM) mode, which means that the light could be well confined in the prepared film.     

Effect of oxygen vacancy variation on the photo-assisted degradation and structural phase transition of oxygen defective Ba(Fe,Co)O3−x

The different effect of oxygen vacancy variation on photo-assisted degradation effect and structural phase transition of oxygen defective Ba(Fe,Co)O_3−x in dye degradation were investigated via comparative studies. The samples of perovskite BaFeO_3−x and BaCoO_3−x were synthesized at 700 °C by citrate sol-gel method. Samples synthesized above 700 °C show oxygen deficiency. With oxygen vacancy increasing, the BaFeO_3−x becomes instable, whereas BaCoO_3−x improves the stability. The instability is due to CO₂ adsorption activity of oxygen vacancies, and then this may make negative effects on their photo-assisted degradation effect. So finally, the oxygen vacancies take different effects on photo-assisted degradation effect of Ba(Fe,Co)O_3−x.     

Influence of oxygen pressure on elastic strain and excitonic transition energy of ZnO epilayers prepared by pulsed laser deposition

High quality ZnO epilayers (χ_min ∼ 10%) were prepared on Al₂O₃ (0 0 0 1) substrates at a temperature of 750 °C by pulsed laser deposition (PLD) with oxygen pressure of 0.015, 0.15, 1.5, and 15 Pa. The best crystalline quality and strongest intensity of UV photoluminescence were observed on ZnO layer with oxygen pressure of 15 Pa. It is probable due to the higher oxygen pressure lessens oxygen deficiency in the film. The tetragonal distortion e_T, which is caused by elastic strain in the epilayer, was determined by Rutherford backscattering/channeling. It reduces as a whole (from 0.93 to 0.65%) with the increase of oxygen pressure from 0.015 to 15 Pa and the excitonic transition energy simultaneously shows a weak blue shift.     

Photoluminescence of GaN microcrystallites prepared by a new solvothermal process

GaN microcrystallites have been prepared by a solvothermal process. The influence of the synthesis temperature on the crystallinity of the resulting GaN has been studied on three samples, prepared at 400, 600 and 800°C in the same pressure conditions (150 MPa) and duration (6 h). The resulting powders were characterized by several techniques: X-ray diffraction to evaluate the reaction rate, scanning electron microscopy (SEM) to determine the morphology and size of the microcrystallites and photoluminescence to evaluate the quality of the powders.     

Spark plasma sintering of BiFeO3

Dense BiFeO₃ ceramics were prepared by a novel spark plasma sintering (SPS) technique. The sintering was conducted at temperatures ranging from 675 to 750 °C under 70 MPa pressure. A bulk density value up to 96% of theoretical density was achieved in the process. This contrast to around 90% of the theoretical density achieved by conventional sintering at around 830 °C. It was found that the tendency to form unwanted Bi₂Fe₄O₉ phase is higher at a high sintering temperature for SPS. The dielectric and ferroelectric properties also improved (with respect to conventionally sintered sample) for spark plasma-sintered samples.     

Enhancement of paint adhesion to cold rolled steel in salt bath by low temperature Ar-H2 plasmas

This study investigates the enhanced adhesion of paint to cold rolled steel (CRS) in salt bath by Ar-H₂ plasmas. It is found that the surface treatment on CRS, prior to painting, by low temperature plasma cleaning with argon-hydrogen plasmas at room temperature (23 °C), can be used for improving the adhesion of paint to CRS in salt bath. The tape test (ASTM 3359 Method) demonstrated this improvement, with a rating of “0” for untreated CRS for aging at a 3.5 wt% NaCl solution for 6 days and “5” for argon-hydrogen plasma-cleaned CRS at certain plasma conditions even for aging at a 3.5 wt% NaCl solution for 6 days. The adhesion performance of paint to CRS in salt bath is highly dependent on the surface characteristics of the CRS and the work of adhesion of paint to CRS.     

Transmission electron microscopy characterization of Al2Cu precipitate growth kinetics by in situ heat treatment

Growth kinetics of the Al₂Cu (θ) precipitate in an Al-1.5Cu alloy thin film were characterized in situ using transmission electron microscopy (TEM). The sizes of θ precipitates during isothermal growth in TEM were measured during aging at 250, 275 and 300 °C. The results of precipitate growth were analyzed based on the model of the “collector plate mechanism” for bulk alloys. The lengthening of the θ precipitate in thin film varies as t^0.29 for short annealing times (up to ∼10-20 min) at temperatures between 250 and 300 °C. This is in good agreement with the analysis in bulk alloys. For longer annealing time, however, the t^0.29 time law does not fit as the distances of Cu volume diffusion exceed one half of the film thickness.     

Effects of preheating temperature on cold cracks,microstructures and properties of high power laser hybrid welded 10Ni3CrMoV steel

Laser hybrid welding has become one of the most promising welding methods for high strength low alloy steels due to combining the advantage of the laser and arc. A novel Y-groove cold cracking test adapted to laser hybrid welding is designed to assess the weldability of 10Ni3CrMoV steels at room temperature and different preheating temperatures. The experimental results show that the orientation of the predominant root cracks generally follows the contour of the fusion line. As the temperature increases from 25 °C to 150 °C, at first the root crack rate decreases and then slightly increases at 150 °C. The root crack rate obtained at 120 °C is the lowest. The fracture model changes from a brittle cleavage fracture to a mixture fracture with quasi-cleavage facets and dimples. The thermal cycle curves of laser hybrid welding obtained by temperature measurement systems are used to evaluate the crack resistance and microstructure transformation. The microstructures of welded joints obtained at different temperatures are analyzed by optical microscope (OM). The results reveal that the microstructures of the coarse grained region and the fusion zone at 120 °C have higher cold crack resistance and good impact toughness. Mechanical properties of the welded joint obtained at 120 °C and 150 °C are comprehensively evaluated by microhardness test, uniaxial tensile test and charpy V-notch impact test with side notches. Fractographs of the impact specimens are studied by scanning electron microscopy (SEM). The test results show that the welded joints obtained at 120 °C have satisfactory mechanical properties that can meet the technical requirements for shipbuilding industry.     

Deposition of hydroxyapatite thin films by Nd:YAG laser ablation: a microstructural study

Hydroxyapatite (HA) thin films has been successfully deposited by Nd:YAG laser ablation at λ = 532 nm. The morphology and microstructure of the deposited layers was studied by scanning electron microscopy (SEM), transmission electron microscopy (TEM) and high resolution electron microscopy (HREM). Polycrystalline HA films were directly obtained with the substrate at 300 °C and without introducing water vapors in the deposition chamber. Electron paramagnetic resonance (EPR) measurements show that the oxygen stoichiometry in the HA films is also maintained. Depositions performed at λ = 335 nm laser wavelength and 300 °C substrate temperature resulted in polycrystalline layers of mixed composition of HA and tricalciumphosphate (TCP).     

Allyloxy-modified starch with low degree of substitution for fiber reinforced thermoset starch composites

In the present work dough moulding compound premixes of allyl glycidyl ether modified (AGE)-potato starch, (DS) = 0.2, has been prepared and tested for its fiber reinforced composite properties. The AGE-starch was hydrolyzed with α-amylase under neutral condition for 6 h at 45 °C for improved process ability. The grafting and hydrolytic scission was confirmed by nuclear magnetic resonance (NMR) and size exclusion chromatography (SEC), respectively. Homogeneous composite premixes of AGE-starch, wood fibers, various amount of glycerol and ethylene glycol dimethacrylate were successfully mixed with a Brabender-kneader at 55 °C and cured by compression molding at 150 °C using 2 wt% of dibenzoyl peroxide. Adding 5 wt% of glycerol did not reduce the ultimate strength of the composites; 10% glycerol reduced the strength from 60 MPa to 40 MPa, and 16% glycerol to 14 MPa. The results with 5 wt% glycerol are comparable with earlier achieved results. The water absorption rate increased with increased glycerol content and the mechanical strength of the composites was lost completely when the moisture uptake reached 15 wt%.     

Influence of fluidized sand bed heat treatment on the performance of Al–Si cast alloys

The present study was undertaken to arrive at a better understanding of the effects of solution heat-treatment time and melt treatment on the microstructure and tensile properties of T6-tempered A356.2 and B319.2 cast alloys heat treated using a fluidized sand bed furnace (FB) as opposed to a conventional convection furnace (CF). The alloys investigated were subjected to solution heat treatment at 530 °C and 495 °C, respectively, for times ranging from 0.5 to 24 h, warm water quenching, and conventional T6 aging at 155 °C and 180 °C, respectively, for times of 0.5, 1, 5, 8 and 12 h. The results revealed that the tensile strength of these alloys is more responsive to an FB heat treatment than to a CF treatment for solution treatment times of up to 8 h. A significant increase in strength is observed in the FB heat-treated samples after short aging times of 0.5 h and 1 h, the trend continuing up to 5 h. Analysis of the tensile properties in terms of quality index charts showed that both modified and non-modified 319 and 356 alloys display the same quality, or better, after only 2 h treatment in a fluidized bed compared to 10 h using a CF treatment. The 319 alloys show signs of overaging after 8 h of aging using a CF, whereas with an FB, overaging occurs only after 12 h. The Si particle characteristics of the alloys investigated show that the smallest particle size is obtained after solution heat treatment using a fluidized sand bed, the optimum solution heat-treatment time being 0.5 h for modified alloys, and up to 5 h for non-modified alloys.     

Novel hydrothermal synthesis method for tobermorite fibers and investigation on their thermal stability

Tobermorite fibers have been successfully synthesized by hydrothermal reaction at 200°C under the pressure of 2 MPa after 3-10 h using a Ca(II)-EDTA complex precursor. XRD patterns, TG-DTA analysis, and SEM observations show that the products are needle-like tobermorite fibers, which have diameter, length, and aspect ratio in the range of 0.1-10, 40-100, and 20-80 μm, respectively. The fibers can maintain their shapes up to 1150°C during the heat treatment.     

Synthesis of spherical LiMnPO4/C composite microparticles

Spherical LiMnPO₄/C composite microparticles were prepared by a combination of spray pyrolysis and spray drying followed by heat treatment and examined as a cathode material for lithium batteries. The structure, morphology and electrochemical performance of the resulting spherical LiMnPO₄/C microparticles were characterized by X-ray diffraction, field-emission scanning electron microscopy, transmission electronic microscopy and standard electrochemical techniques. The final sample was identified as a single phase orthorhombic structure of LiMnPO₄ and spherical powders with a geometric mean diameter of 3.65 μm and a geometric standard deviation of 1.34. The electrochemical cells contained the spherical LiMnPO₄/C microparticles exhibited first discharge capacities of 112 and 130 mAh g⁻¹ at 0.05 C at room temperature and 55 °C, respectively. These also showed a good rate capability up to 5 C at room temperature and 55 °C.     

Synthesis of uniform nano-structured lead oxide by sonochemical method and its application as cathode and anode of lead-acid batteries

This paper discusses the results of a research aimed at investigating the synthesis of nano-structured lead oxide through reaction of lead nitrate solution and sodium carbonate solution by the sonochemical method. At the first, lead carbonate was obtained in a synthesized solution and then, after filtration, it was calcinated at the temperature of 320 °C so that nano-structured lead oxide can be produced. The effects of different parameters on particle size and morphology of final lead oxide powder were optimized by a “one at a time” method. The prepared lead oxide powder was characterized by scanning electron microscopy (SEM), transmission electron spectroscopy (TEM) and X-ray diffraction (XRD). Under optimum conditions, uniformed and homogeneous nano-structured lead oxide powder with more spongy morphology and particle size of 20-40 nm was obtained. The synthesized lead oxide, as anode and cathode of lead-acid batteries, showed an excellent discharge capacity (140 mA h/g).     

Porous alumina/zirconia layered composites with unidirectional pore channels processed using a tertiary-butyl alcohol-based freeze casting

Symmetric three-layer porous alumina/zirconia composites with controlled “designer” pore structure have been prepared by a tertiary-butyl alcohol-based freeze casting and sintering at 1400–1500 °C in air. Unidirectional aligned macropore channels were developed over a long range by controlling the solidification direction of tertiary-butyl alcohol solvent; in this case, they were surrounded by more dense structured walls. In layered composite, the bottom layer consisted of small sized pore channels (∼11 μm in diameter) compared with the middle and the top layer, due to the comparatively rapid velocity of the TBA crystal growth during solidification. The compressive strength (63–376 MPa) of the sintered porous layered composite remarkably increased as the porosity decreased (64–32%).     

Combustion synthesis and characterization of NiCuZn ferrite powders

In this paper, the feasibility of synthesizing NiCuZn ferrite powders by combustion synthesis (CS) reaction is demonstrated through igniting the mixtures of iron, iron oxide, copper oxide, zinc oxide and copper carbonate under different oxygen pressure values. The ferrite powders produced directly from the CS reaction and after annealing at 800 °C for 2 h are characterized by XRD, SEM, XPS and VSM. The results show that the spinel phase in the combustion products increases with the decrease of the diluent content and the increase of the oxygen pressure. Heating the as-synthesized ferrite at 800 °C for 2 h affords pure crystalline NiCuZn ferrite, which possesses better magnetic properties. XPS studies confirm that copper ions in the as-synthesized ferrite are present in the different ionic states of the A- and B-sites, while copper ion is divalent in the B-sites only for the annealed products.     

A non-solvent approach for high-stiffness all-cellulose biocomposites based on pure wood cellulose

All-cellulose composites are commonly prepared using cellulose solvents. In this study, moldable all-cellulose I wood fiber materials of high cellulose purity (97%) were successfully compression molded. Water is the only processing aid. The material is interesting as a “green” biocomposite for industrial applications. Dissolving wood fiber pulps (Eucalyptus hardwood and conifer softwood) are used and the influence of pulp origin, beating and pressing temperature (20–180 °C) on supramolecular cellulose nanostructure is studied by solid state CP/MAS ¹³C NMR. Average molar mass is determined by SEC to assess process degradation effects. Mechanical properties are determined in tensile tests. High-density composites were obtained with a Young’s modulus of up to 13 GPa. In addition, nanoscale cellulose fibril aggregation was confirmed due to processing, and resulted in a less moisture sensitive material.     

Microwave dielectric properties and microstructures of the 11Li2O-3Nb2O5-12TiO2 ceramics with B2O3 addition

The effects of B₂O₃ addition, as a sintering agent, on the sintering behavior, microstructure and microwave dielectric properties of the 11Li₂O-3Nb₂O₅-12TiO₂ (LNT) ceramics have been investigated. With the low-level doping of B₂O₃ (≤2 wt.%), the sintering temperature of the LNT ceramic could be effectively reduced to 900 °C. The B₂O₃-doped LNT ceramics are also composed of Li₂TiO₃ss and “M-phase” phases. No other phase could be observed in the 0.5-2 wt.% B₂O₃-doped ceramics sintered at 840-920 °C. The addition of B₂O₃ induced no obvious degradation in the microwave dielectric properties but increased the τ_f values. Typically, the 0.5 wt.% B₂O₃-doped ceramics sintered at 900 °C have better microwave dielectric properties of ?_r = 49.2, Q × f = 8839 GHz, τ_f = 57.6 ppm/°C, which suggest that the ceramics could be applied in multilayer microwave devices requiring low sintering temperatures.     

Study on the structure and properties of fine-grained alumina fast sintered with high heating rate

Fine-grained alumina was obtained in 2 min by a new densification method based on Self-propagating High-temperature Synthesis plus Quick Pressing (SHS/QP). The sample was densified to more than 99% of theoretical density under a large mechanical pressure (100 MP) and a fast heating rate (1600 °C/min). Compared with the alumina sample obtained by spark plasma sintering (SPS) at lower heating rates (100 or 500 °C/min), almost no grain growth was found in the sample obtained in this work. The microstructure and mechanical properties were studied. Hardness value of 18.6 ± 0.4 GPa and fracture resistance value of 3.4 ± 0.3 MPa m^1/2 were measured for fine-grained alumina of this work. The densification mechanism was discussed.