Effects of TiB2 on microstructure of nano-grained Cu–Cr–TiB2 composite powders prepared by mechanical alloying

Nano-grained CuCr25 and CuCr25–(2 wt%–10 wt%)TiB₂ composite powders were prepared by mechanical alloying method. The milled powders were characterized by SEM, FSEM, EDS, XRD, TEM and HTEM. The results indicate that average grain size of Cu, Cr and TiB₂ are less than 50 nm and each component disperses uniformly. The grain size of Cu and Cr decreased and the lattice distortion increased gradually as the TiB₂ content increased from 2 wt% to 10 wt%. The ultrafine TiB₂ particles play the role of “micro-milling balls” to compact, micro-etch, micro-frict and micro-cut with Cu and Cr so that the grain refinement and lattice strain are promoted.     

Structural and microwave absorption properties of nanostructured Fe–Co alloys

We analyzed nanostructured Fe₆₀Co₄₀ alloy obtained by mechanical alloying using a planetary ball mill. The prepared powders were characterized using X-ray Diffraction (XRD), Laser particle-measurement, scanning electron microscopy (SEM), X band waveguide and cavity resonator associated with Network analyzer. Obtained results are discussed according to milling time.XRD patterns show after 12 h of milling the formation of a disordered solid solution having body-centerd cubic (bcc) structure. After 36 h milling, morphological studies indicated that the average crystallites size is around 13 nm and the particles average diameter is about 3.6 μm. The microwave absorbing characteristic was enhanced between 0 and 54 h of milling (from ?0.8 to ?13.807 dB) with decreasing in the relative dielectric permittivity ε_r.     

Mechanically induced self-propagating reaction and consequent consolidation for the production of fully dense nanocrystalline Ti55C45 bulk material

We employed a high-energy ball mill for the synthesis of nanograined Ti₅₅C₄₅ powders starting from elemental Ti and C powders. The mechanically induced self-propagating reaction that occurred between the reactant materials was monitored via a gas atmosphere gas-temperature-monitoring system. A single phase of NaCl-type TiC was obtained after 5 h of ball milling. To decrease the powder and grain sizes, the material was subjected to further ball milling time. The powders obtained after 200 h of milling possessed spherical-like morphology with average particle and grain sizes of 45 μm and 4.2 nm, respectively. The end-products obtained after 200 h of ball milling time, were then consolidated into full dense compacts, using hot pressing and spark plasma sintering at 1500 and 34.5 MPa, with heating rates of 20 °C/min and 500 °C/min, respectively. Whereas hot pressing of the powders led to severe grain growth (~ 436 nm in diameter), the as-spark plasma sintered powders maintained their nanograined characteristics (~ 28 nm in diameter). The as-synthesized and as-consolidated powders were characterized, using X-ray diffraction, high-resolution electron microscopy, and scanning electron microscopy. The mechanical properties of the consolidated samples obtained via the hot pressing and spark plasma sintering techniques were characterized, using Vickers microhardness and non-destructive testing techniques. The Vickers hardness, Young's modulus, shear modulus and fracture toughness of as-spark plasma sintered samples were 32 GPa, 358 GPa, 151 GPa and 6.4 MPa·m^1/2, respectively. The effects of the consolidation approach on the grain size and mechanical properties were investigated and are discussed.     

Fabrication of transparent Lu3NbO7 by spark plasma sintering

We demonstrated the first successful fabrication of a transparent Lu₃NbO₇ body by spark plasma sintering (SPS). First, Lu₃NbO₇ powder was synthesized by a solid-state reaction of Lu₂O₃ and Nb₂O₅ powders at 1473 K for 7.2 ks and was sintered by SPS at 1723 K for 2.7 ks. The transparent Lu₃NbO₇ body had a cubic defect-fluorite structure and uniform microstructure with an average grain size of 0.77 μm. The transmittance at 550 nm reached 68%.     

Mixture of fuels approach for the solution combustion synthesis of LaAlO3 nanopowders

A modified solution combustion approach was used in the preparation of nanosize LaAlO₃ (～23.6 nm) using mixture of citric acid and oxalic acid as fuels with corresponding metal nitrates. The synthesized and calcined powders were characterized by Fourier transform infra red spectrometry (FTIR), Differential thermal analysis-Thermogravimetry analysis (DTA–TGA), X-ray diffractometry (XRD) and Transmission electron microscopy (TEM). The FTIR spectra show the lower frequency bands at 656 and 442 cm^?1corresponds to metal–oxygen bonds (possible La–O and Al–O stretching frequencies) vibrations for the perovskite structure compound. DTA confirms the formation temperature of LaAlO₃ varies between 830–835 °C. XRD results show that mixture of fuels ratio is influential on the crystallite size of the resultant powders. The average particle size of LaAlO₃-1 as determined from TEM was about 41 nm, whereas for LaAlO₃-2 and LaAlO₃-3 samples, particles are seriously aggregated.     

Photoluminescent emission of Pr3+ ions in different zirconia crystalline forms

Polycrystalline praseodymium doped-zirconia powders were synthesized by crystallization of a saturated solution and annealed in air at T_a = 950 °C. Monoclinic, tetragonal and cubic crystalline phases of zirconia were obtained. EDS studies showed homogeneous chemical composition over all the powders particles and chemical elemental contents in good agreement with the incorporation of Pr³⁺ ion in Zr⁴⁺ sites. XRD patterns showed stabilization of tetragonal and cubic phases at 1.28 and 2.87 at.% of Pr³⁺ doping concentrations, respectively. Both unit cells expand when Pr³⁺ content increases. All samples showed a crystallite size lower than 27 nm. Diffuse reflectance studies exhibited the presence of the 4f5d absorption band of Pr³⁺, and absorption peaks in 440–610 nm region associated with 4f inter-level electronic transitions in Pr³⁺ ion. Low temperature (20 K) photo-luminescent spectroscopic measurements over excitation of 488 nm for praseodymium doped zirconia, showed multiple emission peaks in the 520–900 nm range of the electromagnetic spectrum, associated with typical 4f inter-level electronic transition in Pr³⁺. Incorporation of Pr³⁺ in more than one zirconia crystalline phase and the incorporation in cubic C₂ sites, were observed. Zirconia powders presented significant differences in its emission spectra as a function of the type of crystalline phase compounds.     

Effect of cup and ball types on alumina–tungsten carbide nanocomposite powder synthesized by mechanical alloying

Alumina-based nanocomposite powders with tungsten carbides particulates were synthesized by ball milling WO₃, Al and graphite powders. X-ray Diffraction (XRD) was used to characterize the milled and annealed powders. Microstructures of milled powders were studied by Transmission Electron Microscopy (TEM). Results showed that Al₂O₃–W₂C composite formed after 5 h of milling with major amount of un-reacted W in stainless steel cup. The remained W was decreased to minor amount by increasing carbon content up to 10 wt.%. When milled with ZrO₂ cup and balls, Al₂O₃–W₂C composite was completely synthesized after 20 h of milling with the major impurity of ZrO₂. In the case of stainless steel cup and balls with 10 wt.% carbon, Fe impurity after 5 h of milling (maximum 0.09 wt.%) was removed from the powder by leaching in 3HCl·HNO₃ solution. The mean grain size of the powder milled for 5 h was less than 60 nm. The powder preserved its nanocrystalline nature after annealing at 800 °C.     

Cellulose-precursor synthesis of nanocrystalline Co0.5Cu0.5Fe2O4 spinel ferrites

Nanocrystalline Cu_0.5Co_0.5Fe₂O₄ powders were prepared via a metal-cellulose precursor synthetic route. Cellulose was used as a fuel and a dispersing agent. The resulting precursors were calcined in the temperature range of 450–600 °C. The phase development of the samples was determined by using Fourier transform infrared (FT-IR) spectroscopy and powder X-ray diffraction (XRD). The field-dependent magnetizations of the nanopowders were measured by vibrating sample magnetometer (VSM). All XRD patterns are of a spinel ferrite with cubic symmetry. Microstructure of the ferrites showed irregular shapes and uniform particles with agglomeration. From XRD data, the crystallite sizes are in range of 16–42 nm. Saturation magnetization and coercivity increased with increasing calcining temperature due to enhancement of crystallinity and reduction of oxygen vacancies.     

Fabrication and characterization of Ni–W solid solution alloys via mechanical alloying and pressureless sintering

Ni–W solid solution alloy powders and sintered compacts were fabricated via mechanically alloying and pressureless sintering of powder batches with the compositions of Ni–xW (x = 20, 30, 40 wt.%). The crystallite size of the powders were between 11 nm and 17 nm, which decreased with increasing W contents, where a microhardness value of 6.88 GPa for the Ni powders MM’d for 48 h increased to 9.37 GPa for the Ni40W powders MA’d for 48 h. The MM’d/MA’d powders were sintered at 1300 °C for 1 h under Ar and H₂ gas flowing conditions. X-ray diffraction (XRD) patterns of the sintered Ni, Ni20W and Ni30W samples revealed the presence of only the solid solution phase, whereas the presence of elemental W and Ni₄W intermetallic phase were observed in the XRD patterns of the sintered Ni40W sample. Among all sintered samples, the sintered Ni sample had the highest relative density value of 96.36% and the lowest microhardness value of 1.59 GPa. The relative densities of the sintered samples decreased with increasing W amounts, contrary to microhardness values which increased with W contents. Moreover, microstructural characterizations via scanning electron microscope and electron backscatter diffraction, room temperature compression tests and sliding wear experiments were conducted in order to reveal the effects of W contents on the properties of the sintered Ni–W alloys.     

Green light-emitting Lu3Al5O12:Ce phosphor powders prepared by spray pyrolysis

Green light-emitting Lu_2.985Al₅O₁₂:Ce_0.015 (LuAG:Ce) phosphor powders are prepared by spray pyrolysis. The only crystallized phase in the precursor powders and post-treated powders at temperatures below 800 °C is Lu₂O₃ and the other components are amorphous. Phase pure cubic garnet LuAG:Ce phosphor powders are obtained by post-treatment at 1000 °C. Phosphor powders post-treated at temperatures below 1400 °C retain the spherical shape of the precursor powders. The mean crystallite sizes of phosphor powders post-treated at 1200, 1400, and 1500 °C are 30, 46, and 54 nm, respectively. The excitation spectra contain two bands: a weak band with the maximum peak at 345 nm and a strong broad band in the spectral range from 400 to 490 nm with the maximum peak at 455 nm. The LuAG:Ce phosphor powders have broad emission spectra between 480 and 600 nm, with the maximum peak intensity located at 507 nm. The photoluminescence intensity of the phosphor powders post-treated at 1400 °C is 84.2% of that of the powders post-treated at 1500 °C.     

Hierarchical architecture of Bi12TiO20 via ethylene glycol-mediated synthesis route

Hierarchical architecture of cubic sillenite bismuth titanate (Bi₁₂TiO₂₀) is successfully synthesized using simple ethylene glycol-mediated self-assembly; followed by calcination under air at 600 °C for 30 min. The products are characterized using field emission scanning electron microscopy (FE-SEM), fourier transform infrared spectroscopy (FT-IR), thermogravimetric-differential thermal analysis (TG-DTA), and X-ray diffraction (XRD). The reaction time has an effect on the product morphology, which changed from a leaf- and circular plate-like structure to a completely formed hierarchical structure within 2 h. The hierarchical structure of Bi₁₂TiO₂₀, having a size around 3 μm, is composed of 2D twist nanoplates, and each twist nanoplate has a thickness around 10–30 nm.     

The synthesis and photoluminescence of nanocrystalline Zr0.80Zn0.20O1.80+δ powders via glycine nitrate process

Nanocrystalline Zr_1−xZn_xO_2−x+δ (x = 0, 0.20, 1.00) powders were synthesized by glycine nitrate process route and the Zr_0.80Zn_0.20O_1.80+δ powders were calcined in the temperature range between 500 and 800 °C. An intense UV emission band centered at 382 nm with excitation at 292 nm has been observed in Zr_0.80Zn_0.20O_1.80+δ powders calcined at 600 °C, and X-ray diffraction analysis indicates that the powders exhibit a single phase with cubic ZrO₂ structure with the average grain size is about 7 nm. According to the results of photoluminescence and annealing experiments in different atmospheres, it can be proposed that the intense UV emission band is related to the defect states involving oxygen vacancies. Compared with pure ZrO₂, the incorporation of Zn²⁺ ions enhances UV emission intensity. Our experimental results also show that photoluminescence intensity depends on the concentration of defects and the peak position is related to the crystal phase structure. The novel strong UV emission properties of this material may be very interesting for further application.     

Preparation of nanostructured nickel aluminate spinel powder from spent NiO/Al2O3 catalyst by mechano-chemical synthesis

In this paper, the possibility of mechano-chemical synthesis, as a single step process for preparation of nanostructured nickel aluminate spinel powder from NiO/Al₂O₃ spent catalyst was investigated. Powder samples were characterized in terms of composition, morphology, structure, particle size and surface area using complementary techniques such as X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), differential thermal analysis (DTA) and volumetric adsorption of nitrogen. It was found that formation of spinel was possible after 60 h of milling with no heat treatment. Additionally, influence of mechanical activation on the heat treatment temperature was discussed. It was observed that heat treatment of 15 h milled sample at 1100 °C is enough to produce nickel aluminate spinel. A product of direct mechanical milling showed higher value of surface area (42.3 m²/g) and smaller crystallite size (12 nm) as compared to the heat treated product.     

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.     

Effects of β-alanine on morphology and optical properties of CoAl2O4 nanopowders as a blue pigment

In this paper, we have synthesized cobalt aluminate (CoAl₂O₄), nanopowders as blue pigments by the combustion method, which metal nitrates were used as precursor materials and mixture of urea and glycine as fuel. The effect of β-alanine weight percentage as a novel excess fuel on some physical characteristics (e.g. crystallite size and color) of powders has been investigated. The synthesized powders were characterized by means of X-ray diffraction (XRD), Field emission scanning electron microscopy (FE-SEM), Transmission electron microscope (TEM), Fourier transform infrared (FT-IR) and Ultraviolet–visible (UV–Vis) spectroscopies. XRD patterns and FT-IR spectra confirmed the formation of pure nanocrystalline CoAl₂O₄ powders after calcination of the metal-fuel gel precursors at 600 °C for 2 h. Optical band gap of 2.3 eV observed for the prepared powders. The crystallite sizes were estimated of 20–30 nm by means of TEM images and Williamson–Hall method. UV–Vis spectra of the blue metal oxides were characteristics of Co²⁺ metal ions located in tetrahedral sites. CIE L¹a¹b¹ chromatic coordinates indicated that the bluest color was obtained for β-alanine = 5.5 and 35.6 wt.%.     

Characterization of phases in a Mg–6Gd–4Sm–0.4Zr (wt.%) alloy during solution treatment

Phases in as-cast and solution-treated Mg–6Gd–4Sm–0.4Zr (wt.%) alloy have been characterized using transmission electron microscopy in this paper. The intermetallic phase in as-cast microstructure has a face centered cubic crystal structure (a = 2.2879 nm) with a composition of Mg_6.2(Sm_0.56Gd_0.44) and was dissolved after solution treatment. A particulate phase with a face centered cubic crystal structure (a = 0.5502 nm) was found in the solution-treated microstructure and suggested to already exist in as-cast sample as the nucleus for its further growth during solution treatment.     

Mechanical synthesis of nanostructured titanium–nickel alloys

The methods of mechanically assisted synthesis and mechanical alloying are used to obtain nanostructured TiNi shape-memory alloys. A stoichiometric mixture of Ti and Ni powders was subjected to intense mechanical treatment in a planetary ball mill. It was shown that after 30 h milling, the synthesis of the product with a mean particle size of 20–30 nm proceeded at 550 °C. XRD data show mainly the presence of TiNi, Ti₂Ni and TiNi₃ phases. Prolongation of the milling process up to 40 h leads to direct synthesis of a product with a similar phase composition. SEM and TEM analyses are used to study morphological changes of reagent and product particles in the course of mechanical treatment and after the synthesis of products. The mechanochemical synthesis routes are compared with the traditional method of thermal synthesis. The advantages of the mechanochemical methods of synthesis of nanostructured products and obtaining Ti–Ni powders with a high sinterability are also discussed. It was shown that after cold pressing and sintering at 800 °C, compacts containing even distributed pores with a mean size of 1 μm were obtained. TiNi bodies with similar structural peculiarities are suitable for the purposes of implantology.     

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.     

Combustion synthesis of WC powder in the presence of alkali salts

This paper deals with the formation of tungsten carbide sub-micrometer powders from WO₃ + Mg + C + sodium salts (NaCl, Na₂CO₃) system by combustion synthesis technique. The powders were characterized by XRD and FESEM. X-ray data demonstrate the superiority of the NaCl + Na₂CO₃ combined mixture in the WC formation process. Single phase, sub-micrometer WC powders were synthesized at temperatures as low as 1600 °C. The roles of sodium salts in combustion process were discussed and chemical mechanism of WC formation was proposed. WC powder produced by salt-assisted combustion synthesis technique has a size 0.2–3 μm, crystalline shape and low agglomeration degree.     

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.