Synthesis of spherical NiO nanoparticles through a novel biosurfactant mediated emulsion technique

Spherical nickel oxide nanoparticles were synthesized by microemulsion technique using rhamnolipids as the surfactant along with n-heptane and water. Nickel hydroxide (Ni(OH)₂) particles were first formed which were then calcined to obtain nickel oxide (NiO) particles. Scanning Electron Microscopy (SEM) studies revealed that the synthesized nickel hydroxide particles were spherical in shape with stacked lamellar sheets. Nickel hydroxide was converted to nickel oxide by calcinations at 600 °C for 3 h and was confirmed by X-ray Diffraction (XRD) analysis. Transmission Electron Microscopy (TEM) showed that the nickel oxide particles were crystalline and of uniform size. The effect of pH on particle size was investigated and it was found that the particle size decreased from 86 ± 8 nm at pH 11.6 to 47 ± 5 nm at pH 12.5. A novel method using rhamnolipid biosurfactant for microemulsion synthesis has been demonstrated which offers an eco-friendly alternative to conventional microemulsion technique based on organic surfactants.     

Mg–Al and Zn–Fe layered double hydroxides used for organic species storage and controlled release

Layered double hydroxides (LDH) containing (Mg and Al) or (Zn and Fe) were prepared by coprecipitation at constant pH, using NaOH and urea as precipitation agents. The most pure LDH phase in the Zn/Fe system was obtained with urea and in Mg/Al system when using NaOH. The incorporation of phenyl-alanine (Phe) anions in the interlayer of the LDH was performed by direct coprecipitation, ionic exchange and structure reconstruction of the mixed oxide obtained by the calcination of the coprecipitated product at 400 °C. The reconstruction method and the direct coprecipitation in a medium containing Phe in the initial mixture were less successful in terms of high yields of organic–mineral composite than the ionic exchange method. A spectacular change in sample morphology and yield in exchanged solid was noticed for the Zn₃Fe sample obtained by ionic exchange for 6 h with Phe solution. A delivery test in PBS of pH = 7.4 showed the release of the Phe in several steps up to 25 h indicating different host–guest interactions between the Phe and the LDH matrix. This behavior makes the preparation useful to obtain late delivery drugs, by the incorporation of the anion inside the LDH layer.     

Fabrication of NiO/YSZ anode material for SOFC via mixed NiO precursors

NiO/YSZ anode material with 45 wt.% NiO for SOFC was synthesized by surface-modification of YSZ powder with mixed nickel oxide precursors. YSZ was treated with acidic nickel nitrate and then followed by basic nickel carbonate. Such prepared NiO/YSZ precursor showed nano-size homogeneous mixture upon calcination at 800 °C. The mixture was ground and subjected to calcination at 1200 °C to give rise to agglomerate-free NiO/YSZ composite powder with particle size of ∼ 0.4–0.7 μm. The composite powder was analyzed by XRD, zetapotential measurements, and SEM. The composite powder produced the Ni/YSZ cermet of homogeneous microstructure with a rigid YSZ skeleton, porosity of 33%, and an electrical conductivity of ∼ 430 S/cm at 800–1000 °C, which is much higher than that (∼ 180 S/cm) prepared by a conventional mixed oxide process.     

Synthesis and characterization of xTiO2(1 − x)α-Fe2O3 magnetic ceramic nanostructure system

Rutile-doped hematite xTiO₂(1 ? x)α-Fe₂O₃ (x = 0.0–1.0) nanostructures were synthesized using mechanochemical activation by ball milling. Their complex structural, magnetic and thermal properties were characterized by X-ray diffraction, Mössbauer spectroscopy and simultaneous DSC–TGA. XRD patterns yielded the dependence of lattice parameters and grain size as a function of ball milling time. For the molar concentrations x = 0.1 and 0.3, the Mössbauer spectra were fitted with one, two, three or four sextets, corresponding to the degree of Ti ion substitution of Fe ions in hematite lattice. After 12 h of ball milling, the completion of Ti ion substitution of Fe ions in hematite lattice occurs for x = 0.1 and 0.3. For x = 0.5 and 0.7, Mössbauer spectra fitting required sextets and a quadrupole-split doublet, representing Fe ions substituting Ti ions in the rutile lattice. The completion of Fe ion substitution of Ti ions in rutile lattice was not observed, as indicated by XRD patterns and Mössbauer spectra for these two molar concentrations. Simultaneous DSC–TGA measurements revealed that the mechanochemical activation by ball milling has a strong effect on the thermal behavior of this nanostructure system. The enthalpy dropped dramatically after 2 h of milling time, indicating the strong solid–solid interactions between TiO₂ and α-Fe₂O₃ after ball milling. The change in weight loss of hematite was caused by the decrease of grain size and ion substitutions between Fe and Ti after mechanochemical activation.     

Copper remediation by Eichhornia spp. and sulphate-reducing bacteria

Eichhornia spp. biomass was collected from Chandola Lake, Ahmedabad, Gujarat, India. Point of zero charge of the biomass was pH 7.3. Flask study showed pH 5 and 2–3 h contact time as optimum conditions for copper sorption with 67.25% copper removal. At the end of 24 h of contact time, copper removal reached to 85.0%, from 100 ppm copper containing solution. Copper loading capacity of the biomass ranged between 9.9 and 28.5 mg g^?1 of biomass. To understand the interaction among pH, temperature, presence of nickel and zinc in the system, 2⁴ factorial experiment was performed. Under the experimental conditions pH and interactions between pH–nickel, temperature–pH and temperature–pH–nickel–zinc were found to be significant with 60–74.7% copper removal. Langmuir isotherm was better fit as compared to Freundlich isotherm and pseudo-second order equation gave R² of 0.999 for biosorption kinetic of Eichhornia biomass. Reactor study showed 90% overall copper removal from 24 L of copper containing waste studied and sulphate-reducing bacteria played a significant role. SEMquant element analysis showed increase from 41.66% to 53.93%, 1.02–19.73% and 0.0–12.39% of chloride, aluminium and copper respectively in the loaded biomass as compare to unexposed biomass.     

Synthesis and characterization of silica core/nano-ferrite shell particles

Core/shell particles were synthesized by assembling oppositely charged ferrite (Fe₃O₄ or NiFe₂O₄) nanoparticles on the surface of monodispersed silica core particles (having size ～0.4 μm) prepared by hydrolysis and condensation of tetraethylortosilicate. Optimal conditions for synthesis of silica core/nano-Fe₃O₄ shell particles were found at pH ～ 5.4. The obtained particles have superparamagnetic behavior above a blocking temperature of ≈25 K, which make them very attractive for a broad range of biomedical and bioengineering applications. Incorporation of nickel into ferrite structure could not be achieved at lower pH value, so functionalization of core particles was required. Incorporation of nickel into ferrite structure was successful at pH above 7, however at higher pH the formation rate of nickel–ferrite particles becomes very fast and the self-aggregation dominates the competing formation of the nickel–ferrite shell. Because of that the self-aggregation was prevented by surface modification of nickel–ferrite nanoparticles with citric acid before their deposition on the functionalized silica core and homogenous and continuous NiFe₂O₄ shell was finally obtained.     

Synthesis of nanometer-sized ceria particles by alternating current electrolysis of aqueous solution

Ceria particles in an average size range from 8 to 70 nm were synthesized from cerium nitrate solutions by electrolysis at AC 0.1–10 Hz using platinum wire electrodes at 25–80 °C. The produced ceria particles dissolved in low pH solutions (pH 1.1–2.7) at a longer electrolysis time (>12 h), which caused the decrease of particle size. Increase of the concentration of Ce³⁺ ions and increase of the electrolysis temperature were effective to enhance the particle yield. Small growth of particles (10–20 nm) was measured when the electrolysis temperature was increased to 60–80 °C. When the applied frequency was increased, the particle size decreased. A theoretical equation of particle size as functions of Ce³⁺ ion concentration, electrolysis temperature and applied frequency was derived. The experimental results were in accordance with the prediction from the theoretical model.     

Synthesis and dispersion of hydroxyapatite nanopowders

Spherical, rod and fibroid hydroxyapatite [HAp, Ca₁₀(PO₄)₆(OH)₂] nanoparticles were prepared and dispersed in aqueous media. Temperature and solution pH were the key factors to synthesis of different morphology and crystallinity. Processing conditions were selected from ternary diagram of pH, temperature and Ca:P ratio. High hydroxyl ion concentration (12.25 ≥ pH ≥ 10.5) and low temperature (298 K) favored isotropic non-confined spherical particles, intermediate concentration (9.5 ≥ pH ≥ 7.75) and low temperature (303 K) initiated the anisotropic growth of rod shaped particles but low concentration (7 ≥ pH ≥ 5.25) and high temperature (353 K) accelerated one-dimensional fibroid morphology. The dispersed HAp–citrate complex exhibited a constant zeta potential and size distribution for six months.     

Co–Pt–W thin films electrodeposited from sulphate–gluconate baths

Co–Pt–W magnetic thin films were electrodeposited from gluconate baths. Electrochemical characterization (polarization behaviors and transient curves), microstructure and magnetic properties were investigated. It turned out that increase in gluconate concentration and bath pH shifted the deposition potential to more negative potentials. Microstructure of electrodeposited Co–Pt–W thin films was affected by the bath pH and gluconate concentration enormously. Samples obtained from Co–sulphate–gluconate at pH 8.0 and gluconate concentration 0.3 mol L^?1 exhibited single hcp phase with strong (0 0 1) PO. VSM and MFM measurement showed that perpendicular magnetic anisotropy occurred in the Co–Pt–W thin films prepared under these conditions.     

Preparation of biomorphic porous calcium titanate and its application for preconcentration of nickel in water and food samples

Biomorphic porous nanocrystalline-calcium titanate (SPCTO) was successfully prepared using the sol–gel method and with sorghum straw as the template. Characterization was conducted through XRD, SEM and FTIR. The ability of SPCTO to adsorb nickel ion in water was assessed. Elution and regeneration conditions, as well as the thermodynamics and kinetics of nickel adsorption, were also investigated. The result showed that the sorbent by the sol–gel template method was porous and has a perovskite structure with an average particle diameter of 26 nm. The nickel ion could be quantitatively retained at a pH value range of 4–8, but the adsorbed nickel ion could be completely eluted using 2 mol L^? 1 HNO₃. The adsorption capacity of SPCTO for nickel was found to be 51.814 mg g^? 1 and the adsorption behavior followed a Langmuir adsorption isotherm and a pseudo-second-order kinetic model. The enthalpy change (ΔH) of the adsorption process was 33.520 kJ mol^? 1. At various temperatures, Gibbs free energy changes (ΔG) were negative, and entropy changes (ΔS) were positive. The activation energy (E_a) was 25.291 kJ mol^? 1 for the adsorption. These results demonstrate that the adsorption was an endothermic and spontaneous physical process. This same method has been successfully applied in the preconcentration and determination of nickel in water and food samples with good results.     

Effects of substrate parameters on structure and optical properties of ZnO thin films fabricated by pulsed laser deposition

Highly oriented zinc oxide thin films have been grown on quartz, Si (1 1 1) and sapphire substrates by pulsed laser deposition (PLD). The effect of temperature and substrate parameter on structural and optical properties of ZnO thin films has been characterized by X-ray diffraction (XRD), atomic force microscopy (AFM), optical transmission spectra and PL spectra. The experimental results show that the best crystalline thin films grown on different substrate with hexagonal wurtzite structure were achieved at growth temperature 400–500 °C. The growth temperature of ZnO thin film deposited on Si (1 1 1) substrate is lower than that of sapphire and quartz. The band gaps are increasing from 3.2 to 3.31 eV for ZnO thin film fabricated on quartz substrate at growth temperature from 100 to 600 °C. The crystalline quality and UV emission of ZnO thin film grown on sapphire substrate are significantly higher than those of other ZnO thin films grown on different substrates.     

Torsional fatigue with axial constant stress for Sn–3Ag–0.5Cu lead-free solder

A series of multiaxial ratcheting–fatigue interaction tests have been carried out on Sn–3Ag–0.5Cu lead-free solder specimens. All tests were conducted under cyclic shear strain with the constant axial stress at the room temperature with the shear strain rate of 5 × 10⁻³ s⁻¹. It was found that the ratcheting strain increased with increasing axial stress and shear strain amplitude while the fatigue life decreased at the same time. The ratcheting strain rate was linear with axial stress in double logarithmic coordinate. The Ohno–Wang II constitutive model was employed to simulate the stress–strain responses. Several fatigue life prediction models were applied to predict the multiaxial ratcheting–fatigue life of the Sn–3Ag–0.5Cu lead-free solder. The Gao–Chen model which adopted the maximum shear strain and the ratcheting strain rate as the damage parameter predicted the multiaxial ratcheting fatigue life well.     

Synthesis and electrochemical behavior of a new layered cathode material LiCo1/2Mn1/3Ni1/6O2

A new layered type lithium nickel manganese cobalt oxide with the composition of LiCo_1/2Mn_1/3Ni_1/6O₂ was synthesized by using a layered double hydroxides (LDHs) as precursor and solid state reaction method. Phase-pure LiCo_1/2Mn_1/3Ni_1/6O₂ was obtained when the mixed precursors of NiMnCo–LDHs and LiOH·H₂O were calcined at 750 °C for 12 h. It showed discharge capacity of 180 and 148 mAh/g in the first cycle, corresponding to the discharge voltage ranges of 2.5–4.5 and 2.5–4.2 V, respectively, and still delivered 173 and 140 mAh/g after 60 cycles at room temperature, which represented favorable capacity retention upon cycling. This material was expected as a potential alternative of cathode material to be used for Li-ion secondary battery because of its good electrochemical performance and lower synthesis cost.     

A study on in situ growth of TaC whiskers in Al2O3 matrix powder for ceramic cutting tools

In situ growth of tantalum carbide (TaC) whiskers was synthesized in an α-Al₂O₃ matrix powder via a carbothermal reduction technique within a temperature range of 1350–1500 °C in an argon atmosphere. The starting materials consisted of Ta₂O₅, C, Ni and NaCl powders. Different mixing methods and various reaction temperatures were employed. Most of the prepared whiskers were 0.2–0.5 μm in diameter and 5–15 μm in length. The reaction temperature of 1400–1450 °C was suitable for the growth of TaC whiskers and a wet mixing method was beneficial to increase the whisker yield. Some of the whiskers exhibited the needle shape while others exhibited the screw shape. The growth mechanism of the whiskers was a complex mechanism involving a helical screw dislocation mechanism and a vapor–liquid–solid process. No obvious influences of the Al₂O₃ matrix powder on the growth of TaC whiskers were found and the major impurities in the obtained powder were TaC particles, nickel and unreacted carbon.     

Hot shear deformation constitutive analysis and processing map of extruded Mg–12Li–1Zn bcc alloy

The hot shear deformation behavior of an extruded Mg–12Li–1Zn alloy was studied by shear punch test (SPT) in the temperature range 200–300 °C, and in the shear strain rate range 1.2 × 10⁻³–6.0 × 10⁻² s⁻¹. Based on the constitutive analysis of the SPT data, it was found that a sine hyperbolic function could properly describe the hot shear deformation behavior of the material. The activation energy of 108 kJ mol⁻¹ calculated from sine hyperbolic function together with the power-law stress exponents of 3.6–4.7 is indicative of lattice-diffusion-controlled dislocation climb mechanism as an operative deformation mechanism. As a new approach, the shear processing map was developed in order to determine the optimum processing condition, which was found to be 300 °C and 1.2 × 10⁻³ s⁻¹. Domains of the processing map are also interpreted on the basis of the associated microstructural observations. It was found that the post-deformation microstructure is sensitive to the Zener–Hollomon parameter, so that DRX was encouraged with decreasing Z-value.     

Development of encapsulation technique for curcumin loaded O/W emulsion using chitosan based cryotropic gelation

Cryogel based encapsulation of curcumin, an herbal extract, was successfully carried out with a ternary system of colloidal chitosan, κ-carrageenan, and carboxymethylcellulose sodium salt. The effects of chitosan concentration, κ-carrageenan/CMC ratio of the polymer suspension and molecular weight of chitosan on the sol–gel formation were investigated. The effects of cooling rate during freeze-drying and oil phase composition on the encapsulation yield and the release behavior of curcumin from the hydrogel were determined. And so were the effects of pH of the phosphate-buffered media and oil phase composition on the swelling of the specimens. The microstructure of the resulting specimens revealed core-shell nanoparticles (i.e. oil droplet for core and cryogel membrane for shell) entrapped in the cryogel matrix. The encapsulation yield for two types of suspensions was in a range of 83.9 to 99.6% when a high-MW chitosan was used. Controlled release of the encapsulated curcumin in an aqueous system could be maintained for 4 days, and the releasable amount of curcumin was in a range of 41.1 to 59.9%. The encapsulation yield as well as the released pattern and releasable amount of curcumin were significantly influenced by the cooling protocol used during freezing. Irrespective of the introduced oil phase composition, controlled release of curcumin was achievable when the cooling rate was sufficiently high at ? 2.0 °C/min and, interestingly, either a burst release or a first order release could simply be achieved by changing the freezing condition.     

Fish protein hydrolysate production from sardine solid waste by crude pepsin enzymatic hydrolysis in a bioreactor coupled to an ultrafiltration unit

The aims of the study were to optimize the production a fish protein hydrolysate (FPH) by enzymatic hydrolysis of sardine solid waste using crude pepsin, and to scale up the process in a bioreactor coupled to an ultrafiltration unit for product recovery. Results showed that the crude pepsin prepared by autolysis of the mucous membranes of a sheep stomach at optimal conditions (i. e. pH = 1.5–2 and incubation time of 6 h) could be satisfactory used for the enzymatic hydrolysis of fish solid waste. The optimal conditions for enzymatic reaction were: temperature 48 °C, and pH 1.5. The scale up of the enzymatic hydrolysis and the coupling of the reactor an ultrafiltration unit to concentrate the hydrolysate gave good results with a rejection coefficient for the protein hydrolysate product in the range of 90%. The volumetric concentration factor was 2.5, with a permeate flux of 200 L m^? 2 bar^? 1. However, the results also suggest that the ultrafiltration product concentration process may be operating beyond the critical flux at which point irreversible membrane fouling occurs.     

The ambient and high temperature deformation behavior of Al–Si–Cu–Mg alloy with minor Ti,Zr, Ni additions

The principal aim of the present work was to investigate the effects of minor additions of nickel and zirconium on the strength of cast aluminum alloy 354 at ambient and high temperatures. Tensile properties of the as-cast and heat-treated alloys were determined at room temperature and at high temperatures (190 °C, 250 °C, 350 °C). The results show that Zr reacts only with Ti, Si and Al. From the quality index charts constructed for these alloys, the quality index attains minimum and maximum values of 259 MPa and 459 MPa, in the as-cast and solution-treated conditions; also, maximum and minimum values of yield strength are observed at 345 MPa and 80 MPa, respectively, within the series of aging treatments applied. A decrease in tensile properties of ∼10% with the addition of 0.4 wt.% nickel is attributed to a nickel–copper reaction. The reduction in mechanical properties due to addition of different elements is attributed principally to the increase in the percentage of intermetallic phase particles formed during solidification; such particles act as stress concentrators, decreasing the alloy ductility. Tensile test results at ambient temperatures show a slight increase (∼10%) in alloys with Zr and Zr/Ni additions, particularly at aging temperatures above 240 °C. Additions of Zr and Zr + Ni increase the high temperature tensile properties, in particular for the alloy containing 0.2 wt.% Zr + 0.2 wt.% Ni, which exhibits an increase of more than 30% in the tensile properties at 300 °C compared with the base 354 alloy.     

Optical characterization of In2S3–SiO2 nanocomposite thin films synthesized by sol–gel technique

In₂S₃–SiO₂ nanocomposite films (with molar ratios of In₂S₃:SiO₂ = 15:85, 10:90 and 5:95) were prepared on quartz substrates by sol–gel method. Highly confined nanoparticles of In₂S₃ (radius ∼ 1.8–7 nm) were obtained in SiO₂ matrix, indicating SiO₂ to be a good capping agent for the nanoparticles. The films were annealed in air at different temperatures (473–623 K) and characterized by optical, microstructural and photoluminescence measurements. XRD studies showed that annealing in air upto 623 K leads to the formation of oxide free In₂S₃ nanoparticles. The broad Photoluminescence peak observed at ∼353 nm showed a marked blue shift associated with a decrease in intensity with increasing concentration of In₂S₃ in the matrix.     

Synthesis and electrical conductivity of La0.6Sr0.4Ru1−xMgxO3−δ (x = 0–0.6) perovskite solid solution

Sr and Mg were doped at La- and Ru-sites of perovskite oxide LaRuO₃, respectively, to enhance electrical conductivity and catalytic property as a cathode material for a low temperature solid oxide fuel cell. Crystal structure and particle morphology of La_0.6Sr_0.4Ru_1?xMg_xO_3?δ powders (shorten as LSRM) and electrical conductivity of sintered LSRM were studied. LSRM powders (x = 0–0.6) were prepared by co-precipitation method using metal nitrate solutions and ammonium carbonate solution. The freeze-dried powders were heated at 1273 K in air to form LSRM solid solution of orthorhombic structure. The true densities and particle sizes of LSRM solid solution, where valence of Ru was estimated to be 3+, decreased with increasing Mg content. The electrical conductivity of LSRM at x = 0–0.3 was almost independent of temperature and was in a range of 19–360 S cm^?1 at 1073 K. Hole conduction contributed to the high electrical conductivities. LSRM at x = 0.4 and 0.5 was a mixed conductor of oxide ions and holes, and showed a conductivity of 11 S cm^?1 at 1073 K in air. This conductivity decreased at a lower oxygen pressure and reached a constant value below 10 Pa of oxygen pressure.