Template-free hydrothermal derived cobalt oxide nanopowders: Synthesis,characterization, and removal of organic dyes

Pure spinel cobalt oxide nanoparticles were prepared through hydrothermal approach using different counter ions. First, the pure and uniform cobalt carbonate (with particle size of 21.8–29.8 nm) were prepared in high yield (94%) in an autoclave in absence unfriendly organic surfactants or solvents by adjusting different experimental parameters such as: pH, reaction time, temperature, counter ions, and (Co²⁺:CO₃^2?) molar ratios. Thence, the spinel Co₃O₄ (with mean particle size of 30.5–47.35 nm) was produced by thermal decomposition of cobalt carbonate in air at 500 °C for 3 h. The products were characterized by powder X-ray diffraction (XRD), Fourier transform infrared (FTIR), transmission electron microscope (TEM), scanning electron microscope (SEM), and thermal analysis (TA). Also, the optical characteristics of the as-prepared Co₃O₄ nanoparticles revealed the presence of two band gaps (1.45–1.47, and 1.83–1.93 eV). Additionally, adsorption of methylene blue dye on Co₃O₄ nanoparticles was investigated and the uptake% was found to be >99% in 24 h.     

Investigation of mechanical properties of borided Nickel 201 alloy

In this study, the case properties of Nickel 201 alloys, borided in Ekabor-II powder, were investigated by conducting a series of experiments at temperatures of 1173 K for 4 h. The boride layer was characterised by optical microscopy, X-ray diffraction techniques and the micro-Vickers hardness tester. X-ray diffraction analysis of boride layers on the surface of the steels revealed the existence of NiB, Ni₂B, Ni₃B and Ni₄B₃ compounds.The thickness of the boride layer Nickel 201 alloys is approximately 220 μm. The hardness of the boride compounds formed on the surface of the Nickel 201 alloys ranged from 1153 to 1778 HV_0.05, whereas the Vickers hardness values of the untreated Nickel 201 alloys were 180 HV₀₀₅. When the hardness of the boride layer is compared with that of the matrix, the boride layer hardness is approximately ten times greater.     

Microwave-assisted synthesis of BaWO4 nanoparticles and its photoluminescence properties

Single-crystal BaWO₄ nanoparticles have been successfully synthesized under microwave irradiation. The results show that nearly monodisperse BaWO₄ nanoparticles have been successfully prepared without using surfactants. The products were characterized by X-ray powder diffraction (XRD), transmission electron microscopy (TEM), and photoluminescence (PL). The XRD results indicated that the BaWO₄ nanoparticles obtained had a tetragonal unit cell (a = 0.5612, c = 1.2706 nm). The TEM images show that the as-prepared BaWO₄ have good narrow particle-sized distributions containing a number of nanoparticles with uniform sizes. The products show a strong photoluminescence peak at 432–436 nm with the excitation at 365 nm.     

Synthesis of CoO nanoparticles by esterification reaction under solvothermal conditions

A new esterification reaction under solvothermal conditions was first applied to synthesize CoO nanoparticles in this paper. Esterification reaction of cobalt acetate and anhydrous ethanol under solvothermal conditions results in the formation of CoO nanoparticles. The concentrations of cobalt acetate, reaction temperature and surfactant to as-synthesized CoO have been explored. SEM, TEM and XRD were employed to characterize the size, morphology and crystalline structure of the as-synthesized CoO nanoparticles. It is revealed that the FCC-structured CoO nanoparticles are of uniform tetragonal projected shape with good dispersion. Typically, CoO nanoparticles with an average size of 35 nm were obtained at 150 °C for 24 h using 0.08 mol/L solution of Co(CH₃COO)₂·4H₂O in ethanol under solvothermal conditions.     

The influence of preparation conditions on ZrO2 nanoparticles with different PEG–PPG–PEG surfactants by statistical experimental design

In this study mesoporous Zirconia powder with high surface area was prepared by using PEG–PPG–PEG new block copolymer as the non-ionic surfactant. The preparation conditions were optimized by Taguchi method of experimental design and Minitab Software to synthesize high surface area tetragonal-ZrO₂ nanoparticles. The BET surface area of powders was 114–175 m²/gr and the particles size calculated by Deby–Sherrer equation was 5–9 nm. pH = 11, aging time 38 h, Zr molarity 0.03, Surfactant/Zr mole ratio 0.04 and molecular weight 8400 were the best conditions to manufacture ZrO₂ with higher surface area. The sample prepared under optimized conditions was compared to that synthesized by PEG surfactant. XRD patterns of two ZrO₂ samples, hysteresis loop, pore size distribution, BET surface area and SEM results are similar.     

Nanocrystalline Al/Al12(Fe,V)3Si alloy prepared by mechanical alloying: Synthesis and thermodynamic analysis

Al–Al₁₂(Fe,V)₃Si nanocrystalline alloy was fabricated by mechanical alloying (MA) of Al–11.6Fe–1.3V–2.3Si (wt.%) powder mixture followed by a suitable subsequent annealing process. Structural changes of powder particles during the MA were investigated by X-ray diffraction (XRD). Microstructure of powder particles were characterized using scanning electron microscopy (SEM). Differential scanning calorimeter (DSC) was used to study thermal behavior of the as-milled product. A thermodynamic analysis of the process was performed using the extended Miedema model. This analysis showed that in the Al–11.6Fe–1.3V–2.3Si powder mixture, the thermodynamic driving force for solid solution formation is greater than that for amorphous phase formation. XRD results showed that no intermetallic phase is formed by MA alone. Microstructure of the powder after 60 h of MA consisted of a nanostructured Al-based solid solution, with a crystallite size of 19 nm. After annealing of the as-milled powder at 550 °C for 30 min, the Al₁₂(Fe,V)₃Si intermetallic phase precipitated in the Al matrix. The final alloy obtained by MA and subsequent annealing had a crystallite size of 49 nm and showed a high microhardness value of 249 HV which is higher than that reported for similar alloy obtained by melt spinning and subsequent milling.     

Structural and optical properties of chlorinated plasma polymers

Amorphous hydrogenated chlorinated carbon (a-C:H:Cl) films were produced by the plasma polymerization of chloroform–acetylene–argon mixtures in a radiofrequency plasma enhanced chemical vapor deposition system. The main parameter of interest was the proportion of chloroform in the feed, R_C, which was varied from 0 to 80%. Deposition rates of 80 nm min^? 1 were typical for the chlorinated films. Infrared reflection–absorption spectroscopy revealed the presence of C–Cl groups in all the films produced with chloroform in the feed. X-ray photoelectron spectroscopy confirmed this finding, and revealed a saturation of the chlorine content at ~ 47 at.% for R_C ≥ 40%. The refractive index and optical gap, E₀₄, of the films were roughly in the 1.6 to 1.7, and the 2.8 to 3.7 eV range. These values were calculated from transmission ultraviolet–visible-near infrared spectra. Chlorination leads to an increase in the water surface contact angle from ~ 40° to ~ 77°.     

Martensitic transformation behaviors of rapidly solidified Ti–Ni–Mo powders

For the fabrication of bulk near-net-shape shape memory alloys and porous metallic biomaterials, consolidation of Ti–Ni–Mo alloy powders is more useful than that of elemental powders of Ti, Ni and Mo. Ti₅₀Ni_49.9Mo_0.1 shape memory alloy powders were prepared by gas atomization, and transformation temperatures and microstructures of those powders were investigated as a function of powder size. XRD analysis showed that the B2–R–B19 martensitic transformation occurred in powders smaller than 150 μm. According to DSC analysis of the as-atomized powders, the B2–R transformation temperature (T_R) of the 25–50 μm powders was 18.4 °C. The T_R decreased with increasing powder size, however, the difference in T_R between 25–50 μm powders and 100–150 μm powders is only 1 °C. Evaluation of powder microstructures was based on SEM examination of the surface and the polished and etched powder cross sections and the typical images of the rapidly solidified powders showed cellular morphology. Porous cylindrical foams of 10 mm diameter and 1.5 mm length were fabricated by spark plasma sintering (SPS) at 800 °C and 5 MPa. Finally these porous TiNi alloy samples are heat-treated for 1 h at 850 °C, and then quenched in ice water. The bulk samples have 23% porosity and 4.6 g/cm³ density and their T_R is 17.8 °C.     

Sodium gluconate-assisted hydrothermal synthesis,characterization and electrochemical performance of LiFePO4 powders

Nano- and micro-sized LiFePO₄ powders were synthesized by a sodium gluconate (C₆H₁₁NaO₇)-assisted hydrothermal synthesis method at 220 °C for 10 h with pH = 2–7. The resulting powders were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM), and energy-dispersive X-ray spectrometer (EDS). The obtained data showed that the pH of synthesis solution played a key role in the formation of the LiFePO₄ powders with different morphologies, such as ball-like microspheres, irregular microspheres with the agglomerated rods and particles, sphere-like nanoparticles and nano-ellipsoids. The results from electrochemical performance measurements revealed that the charge–discharge cycling characteristics of the samples were strongly dependent on their morphologies. In particular, the ellipsoidal LiFePO₄ nanoparticles with the average size of 70–90 nm showed the highest initial discharge capacity of 150 mA h g⁻¹ at 0.1 C rate, and cycling stability of the ellipsoidal LiFePO₄ nanoparticles was optimum among all the samples prepared due to their dual advantages of high tap density and good diffusion property. The present study offers a simple morphology-controllable route, without carbon coating or doping with supervalent cations, to synthesize and to design high performance cathode materials for lithium-ion batteries.     

Physical and electrochemical study of cobalt oxide nano- and microparticles

Cobalt oxide nanocrystals of size 17–21 nm were synthesized by a simple reaction between cobalt acetate (II) and dodecylamine. On the other hand, micrometric Co₃O₄ was prepared using the ceramic method. The structural examination of these materials was performed using powder X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), and transmission electron microscopy (TEM and HRTEM). XRD studies showed that the oxides were pure, well-crystallized, spinel cubic phases with a-cell parameter of 0.8049 nm and 0.8069 nm for the nano and micro-oxide, respectively. The average particle size was 19 nm (nano-oxide) and 1250 μm (micro-oxide). Morphological studies carried out by SEM and TEM analyses have shown the presence of octahedral particles in both cases. Bulk and surface properties investigated by X-ray photoelectron spectroscopy (XPS), point zero charge (pzc), FTIR and cyclic voltammetry indicated that there were no significant differences in the composition on both materials. The magnetic behavior of the samples was determined using a vibrating sample magnetometer. The compounds showed paramagnetic character and no coercivity and remanence in all cases. Galvanostatic measurements of electrodes formed with nanocrystals showed better performance than those built with micrometric particles.     

High-sensitivity humidity sensor based on SnO2 nanoparticles synthesized by microwave irradiation method

Tin oxide hexagonal-shaped nanodiscs (SnO) and spherical nanoparticles (SnO₂) have been prepared by using a simple household microwave irradiation method with an operating frequency of 2.45 GHz. This technique permits us to produce gram quantity of homogeneous nanoparticles in just 10 min. The crystallite size was evaluated from powder X-ray diffraction (XRD) studies and was in the 20 to 25 nm range. Transmission electron microscopy (TEM) analysis showed that the as prepared SnO form as hexagonal-shaped nanodiscs and upon subsequent annealing at 500 °C for 5 h in air, the SnO gets converted to spherical-shaped nanoparticles of SnO₂. The SnO₂ sample shows good sensitivity towards the relative humidity. The calculated response and recovery time were found to be 32 s and 25 s respectively. These results indicate promising applications of SnO₂ nanoparticles in a highly sensitive environmental monitoring and humidity controlled electronic devices. The samples were further subjected to thermal analyses (TG–DTA) and UV–VIS diffusion reflectance spectroscopy (DRS) studies.     

Influence of temperature, [Ca2+], Ca/P ratio and ultrasonic power on the crystallinity and morphology of hydroxyapatite nanoparticles prepared with a novel ultrasonic precipitation method

Nanocrystalline hydroxyapatite was prepared by a precipitation method with the aid of ultrasonic irradiation using Ca(NO₃)₂ and NH₄H₂PO₄ as source material and carbamide (NH₂CONH₂) as precipitator. The influence of Ca/P molar ratio, precipitation temperature, concentration of Ca²⁺ ([Ca²⁺]) and ultrasonic power on the crystallinity of the nanopowder were systematically investigated by XRD analysis. The size of the as-prepared particles was analyzed using TEM and XRD methods. The results revealed that the monophase hydroxyapatite could be obtained at the following technological conditions: [Ca²⁺] = 0.01–0.1 mol/L, ultrasonic power = 300 W, Ca/P (mol) = 1.2–2.5 and T = 313–353 K. In addition, the acicular and spherical particles could be prepared at different ultrasonic powers of 300 and 200 W, respectively.     

Pack-boriding of Fe–Mn binary alloys: Characterization and kinetics of the boride layers

In this work, the boronizing of Fe–Mn binary alloys at 0.42, 0.76 and 0.94 wt.% Mn was carried out in a solid medium using the powder pack method. In this method, commercial Ekabor-II boron source and activator (ferro-silicon) were thoroughly mixed to form the boriding medium. The samples were boronized in an electrical resistance furnace for exposure times of 2, 4, 6 and 8 h at 1173 K under atmospheric pressure and a series of boronized samples in the temperature range 1073–1373 K for 3 h. After the furnace process, boronized samples were removed from the furnace and cooled in air. Afterwards, the boride layers generated by the pack-boronizing process were characterized by optical microscopy, scanning electron microscopy, XRD analysis, Vickers microhardness and tensile testing. The generated boride layers, showing a saw-tooth morphology, had a surface microhardness in the range 1400–1270 HV0.1. It was shown that the values of yield stresses and ultimate tensile stresses were increased as the Mn content increases in the boronized Fe–Mn binary alloys. In contrast, the values of elongations determined from the stress–strain curves were decreased. Furthermore, it was found that the calculated mean value of the activation energy of boron diffusion was close to 119 J/mol.     

Influence of carbon precursors on thermal plasma assisted synthesis of SiC nanoparticles

Nanosized SiC was synthesized by solid state method using silicon and carbon powders followed by non-transferred arc thermal plasma processing. X-ray diffraction (XRD) analysis revealed that activated carbon has highest reactivity while graphite has lowest activity in the crystallization of SiC through solid state method. The reactivity was dependent on surface area of carbon source and activated carbon with highest surface area (590.18 m² g⁻¹) showed highest reactivity, whereas graphite with least surface area (15.69 m² g⁻¹) showed lowest reactivity. The free silicon content was decreased with increasing reaction time as well as carbon mole ratio. Scanning electron microscope (SEM) study showed that the shape and size of synthesized SiC depends on the shape and size of carbon source. SiC nanoparticles within 500 nm were formed for carbon black while bigger particles (∼5 μm) were formed for activated carbon and graphite. Plasma processing of these solid–solid synthesized SiC resulted into the formation of well dispersed, ultrafine SiC nanoparticles (30–40 nm) without any structural modification. Thermal plasma processing resulted into the increase in crystallite size of SiC.     

Synthesis of cobalt nanoparticles to enhance magnetic permeability of metal–polymer composites

Metallic cobalt nanoparticles were synthesized by hydrogen reduction method. Particles were coated in situ with carbon by adding ethene to reaction flow. Particles were characterized by transmission electron microscopy, energy dispersive X-ray emission, X-ray diffraction, X-ray fluorescence and BET method. The observed cobalt particle size distributions in different cobalt batches produced with unvarying reaction parameters was reproducible: The mean diameter of primary cobalt particle varied only 5% from the mean value of 76 nm in different batches. Increased carbon precursor concentration decreased mean diameter of cobalt particles to 17 nm. The produced nanoparticles were used as filler material in 0–3 type metal–polymer composites. Composite samples with varying filler loading were fabricated with mixing extrusion and injection moulding techniques. The magnetic properties of the fabricated composites were measured up to 1 GHz. In order to analyse the particle distribution in composite matrix and its effect on magnetic properties the microstructure was studied.     

Synthesis of copper and copper(I) oxide nanoparticles by thermal decomposition of a new precursor

The present investigation reports, the novel synthesis of nanoparticles Cu and Cu₂O using thermal decomposition and its physicochemical characterization. The nanoparticles copper powder have been prepared using [Bis(salicylidiminato)copper(II)], [Cu(sal)₂], as precursor. Cu nanoparticles are initially formed and subsequently oxidized to form Cu₂O. Transmission electron microscopy (TEM) analysis demonstrated nanoparticles Cu₂O with an average diameter of about 10 nm. As-prepared copper nano-particles were characterized by X-ray diffraction measurements (XRD), scanning electron microscopy (SEM), energy dispersive analysis of X-rays (EDAX), and Fourier transform infra-red spectroscopy (FTIR). XRD analysis revealed broad pattern for fcc crystal structure of copper metal and cubic cuprite structure for Cu₂O. Optical absorption measured by UV–visible spectroscopy was used to monitor oxidation course of Cu → Cu₂O and to determine the band-gap energy about 2.4 eV for Cu₂O nanoshells.     

Surfactant-free synthesis and electromagnetic properties of Co–Ni–B composite particles

The Co–Ni–B composite particles with different mol ratio of Co to Ni were composited of spheres, spheres in-pair, hierarchical assemblies of dentrites, which were surfactant-free synthesized by chemical reduction method in aqueous solution. The complex permeability of the Co–Ni–B composite particles indicated reverse resonant peak at the frequency range of 8–16 GHz, where the complex permittivity showed the positive resonant peak and the μ_r″ of particles showed negative values, caused by the transformation between electric and magnetic energy. The imaginary parts of relative permeability (μ_r″) of Co–Ni–B composite particles indicated one broad resonant peak over the 2–8 GHz range for the high effective anisotropy. A slight decrease in complex permittivity resulted in an excellent impedance matching property. The Co–Ni–B composite alloy particles with mol ratio of 7:3 exhibited reflection loss less than ?20 dB in frequency range of 4.0–14.5 GHz for the absorber thickness of 1.1–3.2 mm, and an optimal RL of ?32.4 dB was obtained at 12.8 GHz with thickness of 1.2 mm. The broadest bandwidth of reflection loss less than ?10 dB from 13.0 to 17.0 GHz, covering almost the whole Ku-band, was obtained for a thickness of 1.1 mm layer.     

Nanoparticles of the giant dielectric material,calcium copper titanate from a sol–gel technique

The precursor of CaCu₃Ti₄O₁₂ (CCTO) nano particles have been successfully synthesized by sol–gel method at 90 °C. The dried precursor powder was milled and then calcined at 450 °C, 550 °C, 650 °C, 800 °C, 850 °C and 950 °C for 3 h. The phase formation of CCTO was analyzed by step by step using FTIR and XRD. Particle size and shape were evaluated by AFM. The XRD results of the powder calcined at 800 °C indicated the formation of CCTO phase. AFM studies showed that average particle size of the CCTO powder range 90–120 nm. The absorption bands corresponding to vibrations of CaO, CuO and TiOTi were observed at 606, 525 and 463 cm^? 1 using FTIR. The samples sintered at 1040 °C showed the densities as high as 96% of theoretical density. The grain sizes of sintered pellets were determined by FE-SEM. The dielectric properties of prepared samples were studied by LCR meter.     

Continuous float–sink density separation of lump iron ore using a dry sand fluidized bed dense medium

A continuous separator based on float–sink density separation using a gas–solid fluidized bed dense medium was used to upgrade iron ore. The separator has three devices for (A) conveying floaters, (B) recovering floaters, and (C) conveying and recovering sinkers. The optimum speeds of these devices were investigated using density adjusted spheres of the diameter = 30 mm in the range of 2400–3300 kg/m³ in density increments of 100 kg/m³. A mixture of zircon sand and iron powder was used as the fluidized medium to adjust the fluidized bed density to produce a separation density = 2850 kg/m³, a typical separation density for lump iron ore wet separation. The recovery of the spheres as floaters or sinkers depended on the speed of the devices, because the recovery was affected by the number density of spheres directly under the feeder, the local fluidized bed density, and flow currents in the medium derived from the movement of the devices. The optimum speeds were determined to be 3.5 cm/s for (A), 2.0 rpm for (B) and 1.0 cm/s for (C), respectively. Continuous separation experiments were conducted on lump iron ore particles in the size range of +11.1–31.5 mm in the fluidized bed with medium density of 2850 kg/m³ and feed rate of 200 kg/h. Comparison of the feed rate and the recovery rate indicated that the feed and the recovery were in equilibrium after 10 min of operation. The experiments resulted in nearly perfect separation; 98.4% of the ore with density greater than 2850 kg/m³ was recovered. The Fe, Al and Si content of the feed ore particles (before the separation) and the floaters and sinkers (after the separation) was measured using inductively coupled plasma spectrometry. The separator produced an upgrade in iron content of 3.3 wt% and reduced the Al and Si content by 44%.     

Mechanochemical assisted synthesis of B4C nanoparticles

The present work reports on the preparation of boron carbide nanoparticles by the reduction of boron oxide with magnesium in the presence of carbon using the mechanochemical processing. The phase transformation and microstructure of powders during ball milling were investigated by X-ray diffractometry (XRD) and scanning electron microscopy (SEM). The results showed that during ball milling the B₂O₃–Mg–C reacted with a self-propagating combustion mode producing MgO and B₄C compounds. To separate B₄C from the milled powder mixture, an appropriate leaching process was used. After leaching, the purified powder mixture was characterized using XRD and transmission electron microscope (TEM). XRD studies indicated that the prepared particles were single phase crystalline B₄C. Moreover, TEM studies showed the size of B₄C particles were ranging from 10 to 80 nm.