Structural and electrochemical properties of nanostructured nickel silicides by reduction and silicification of high-surface-area nickel oxide

Nanostructured nickel silicides have been prepared by reduction and silicification of high-surface-area nickel oxide (145 m² g^?1) produced via precipitation. The prepared materials were characterized by nitrogen adsorption, X-ray diffraction, thermal analysis, FT-IR spectroscopy, scanning electron microscopy, transmission electron microscopy, magnetic and electrochemical measurements. The nickel silicide formation involves the following sequence: NiO (cubic) → Ni (cubic) → Ni₂Si (orthorhombic) → NiSi (orthorhombic) → NiSi₂ (cubic), with particles growing from 13.7 to 21.3 nm. The nickel silicides are ferromagnetic at room temperature, and their saturation magnetization values change drastically with the increase of Si content. Nickel silicides have remarkably low electrical resistivity and noble metal-like properties because of a constriction of the Ni d band and an increase of the electronic density of states. The results suggest that such silicides are promising candidates as inexpensive yet functional materials for applications in electrochemistry as well as catalysis.     

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.     

Diffusion bonding of titanium alloy to micro-duplex stainless steel using a nickel alloy interlayer: Interface microstructure and strength properties

In the present study, diffusion bonding of titanium alloy and micro-duplex stainless steel with a nickel alloy interlayer was carried out in the temperature range of 800–950 °C for 45 min under the compressive stress of 4 MPa in a vacuum. The bond interfaces were characterised by scanning electron microscopy, electron probe microanalyzer and X-ray diffraction analysis. The layer wise Ni₃Ti, NiTi and NiTi₂ intermetallics were observed at the nickel alloy/titanium alloy interface and irregular shaped particles of Fe₂₂Mo₂₀Ni₄₅Ti₁₃ was observed in the Ni₃Ti intermetallic layer. At 950 °C processing temperature, black island of β-Ti phase has been observed in the NiTi₂ intermetallics. However, the stainless steel/nickel alloy interface indicates the free of intermetallics phase. Fracture surface observed that, failure takes place through the NiTi₂ phase at the NiA–TiA interface when bonding was processed up to 900 °C, however, failure takes place through NiTi₂ and β-Ti phase mixture for the diffusion joints processed at 950 °C. Joint strength was evaluated and maximum tensile strength of ∼560 MPa and shear strength of ∼415 MPa along with ∼8.3% ductility were obtained for the diffusion couple processed at 900 °C for 45 min.     

Structure analysis of aluminium silicon manganese nitride precipitates formed in grain-oriented electrical steels

We report a detailed structural and chemical characterisation of aluminium silicon manganese nitrides that act as grain growth inhibitors in industrially processed grain-oriented (GO) electrical steels. The compounds are characterised using energy dispersive X-ray spectrometry (EDX) and energy filtered transmission electron microscopy (EFTEM), while their crystal structures are analysed using X-ray diffraction (XRD) and TEM in electron diffraction (ED), dark-field, high-resolution and automated crystallographic orientation mapping (ACOM) modes. The chemical bonding character is determined using electron energy loss spectroscopy (EELS). Despite the wide variation in composition, all the precipitates exhibit a hexagonal close-packed (h.c.p.) crystal structure and lattice parameters of aluminium nitride. The EDX measurement of ~ 900 stoichiometrically different precipitates indicates intermediate structures between pure aluminium nitride and pure silicon manganese nitride, with a constant Si/Mn atomic ratio of ~ 4. It is demonstrated that aluminium and silicon are interchangeably precipitated with the same local arrangement, while both Mn^2 + and Mn^3 + are incorporated in the h.c.p. silicon nitride interstitial sites. The oxidation of the silicon manganese nitrides most likely originates from the incorporation of oxygen during the decarburisation annealing process, thus creating extended planar defects such as stacking faults and inversion domain boundaries. The chemical composition of the inhibitors may be written as (AlN)_x(SiMn_0.25N_yO_z)_1 − x with x ranging from 0 to 1.     

Controllable synthesis of nickel dendritic crystals induced by magnetic field

We demonstrated in this paper a simple and easy method for the preparation of dendritic nickel crystals in an external magnetic field in boiling ethylene glycol (EG) solution. The structural features and morphology of the sample were investigated using powder X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The values of saturation magnetization (M_s) and coercivity (H_c) of the dendritic crystals characterized by using a vibrating sample magnetometer (VSM) are 170.3 emu g^?1 and 50.7 Oe, respectively. It was clear that the external magnetic field was the most important factor for controlling the morphology of the product.     

Structure and corrosion resistance of nickel coatings containing tungsten and silicon powders

Ni + W + Si coatings were prepared by nickel deposition from a bath containing a suspension of tungsten and silicon powders. These coatings were obtained at galvanostatic conditions, at the current density of j_dep = − 0.100 A cm^− 2 and at the temperature of 338 K. For determination of the influence of phase composition and surface morphology of these coatings on changes in the corrosion resistance, these coatings were modified in an argon atmosphere by thermal treatment at 1373 K during 1 h. A scanning electron microscope was used for surface morphology characterization of the coatings. The chemical composition of the coatings was determined by EDS and phase composition investigations were conducted by X-ray diffraction. It was found that the as-deposited coatings consist of a three-phase structure, i.e., nickel, tungsten and silicon. The phase composition for the Ni + W + Si coatings after thermal treatment is markedly different. The main peaks corresponding to Ni and W coexist with the new phases: NiW, NiWSi and a solid solution of W in Ni.Electrochemical corrosion resistance investigations were carried out in 5 M KOH, using potentiodynamic and electrochemical impedance spectroscopy (EIS) methods. On the basis of these investigations it was found that the Ni + W + Si coatings after thermal treatment are more corrosion resistant in alkaline solution than the as-deposited coatings. The reasons for this are a reduction in the amount of free nickel and tungsten, the presence of new phases (in particular polymetallic silicides), and a decrease of the active surface area of the coatings after thermal treatment.     

Structure and field emission properties of SnO2 nanowires

SnO₂ nanowires were fabricated using a simple and economical method of rapid heating SnO₂ and graphite powders at 850 °C in a flow of high-purity N₂ as carrier gas. Research by using X-ray diffraction (XRD) indicates that SnO₂ nanowires are primitive tetragonal in structure with the lattice constant a = b = 0.443 nm and c = 0.372 nm. Observations by using scanning electron microscopy (SEM) and transmission electron microscopy (TEM) show that SnO₂ is of nanowire structure. The selected area electron diffraction (SAED) shows that the nanowires are perfect single crystal structure. The Fourier transform infrared (FT-IR) exhibits the difference of nanostructure materials and general materials. The field emission (FE) properties had also been studied.     

Synthesis of nanocrystalline GaN by the sol–gel method

Single-phase wurtzite GaN nanocrystals with an average diameter of 11 ± 3 nm were synthesized by the sol–gel technique from readily available Ga(NO₃)₃. Transmission electron microscopy (TEM) and selected area electron diffraction (SAED) confirmed they had a hexagonal structure and a narrow size distribution of the nanocrystals. X-ray powder diffraction (XRD) and high-resolution transmission electron microscopy (HRTEM) measurement showed that the GaN powder was of single-phase wurtzite structure with a considerable fraction of structural defects such as twin and stacking faults. The IR spectrum showed that only the Ga–N stretch is present at 600 cm⁻¹. The EDX pattern of as-prepared product showed their ratio approximate to 1:1. Room temperature photoluminescence (PL) measurement exhibited the band-edge emission of GaN at about 390 nm and defect emission peak at 610 nm.     

Preparation and characterization of LaNiO3 nanocrystals

Ten to twenty-three nanometers of LaNiO₃ nanocrystals were prepared by glycine combustion method using nickel nitrate and lanthanum nitrate as raw materials, glycine as gelating agent and fuel. The preparation process was monitored by thermogravimetric analysis and differential thermal analysis (TG-DTA); the final products were characterized by X-ray diffraction (XRD), electron diffraction (ED), high-resolution transmission electron microscopy (HRTEM) and scanning electron microscopy (SEM). The effect of thermal treatment temperature on crystal size of the nanocrystals was studied and the activation energy of LaNiO₃ nanocrystals formation during calcinations was calculated to be 41.9 kJ/mol. Moreover, the interplanar distances of d₁₁₀ and d₁₀₁ measured from the TEM images were 0.272 and 0.363 nm, respectively, coinciding with the theoretical values.     

Synthesis and crystallization of lead–zirconium–titanate (PZT) nanotubes at the low temperature using carbon nanotubes (CNTs) as sacrificial templates

Pb(Zr_0.52Ti_0.48)O₃ (PZT) nanotubes with diameters of 80–100 nm and a wall thickness of 15–20 nm were prepared by sol–gel template technique and using multi-walled carbon nanotubes (MWCNT) as sacrificial templates. The coating process of MWCNT with PZT precursor sol and removal of the carbon nanotubes by an interrupt heat treatment were discussed and studied by Raman spectroscopy. Simultaneous thermal analysis (STA) revealed that PZT nanotube crystallized at the low temperature of 410 °C by the significantly low activation energy of crystallization of 103.7 kJ/mol. Moreover, based on the X-ray diffraction (XRD) pattern and selected area electron diffraction pattern the crystal structure of the PZT nanotube was determined as perovskite. High resolution transmission electron microscope (HRTEM) and field-emission scanning electron microscope (FE-SEM) images proved that the final PZT had a tubular structure.     

The effects of Ta on the stress rupture properties and microstructural stability of a novel Ni-base superalloy for land-based high temperature applications

A novel polycrystalline Ni-base superalloy was developed for land-based high temperature applications, such as isothermal forging dies and industrial gas turbines. The alloy possessed surprisingly high stress rupture life of 52 h at 1100 °C/118 MPa which is comparable to the first generation single crystal (SC) superalloy and exhibited good microstructural stability. The effects of Ta addition on the phase change, stress rupture properties and microstructural stability of the alloy were investigated. The results indicated that Ta is a γ′-former and promotes the formation of eutectic γ′. The alloys with ∼7 vol.% eutectic γ′ possess higher stress rupture life at 1100 °C/118 MPa than the alloys with higher ∼20 vol.% eutectic. However, ∼20 vol.% excessive eutectic phases will enhance the stress rupture life at intermediate temperature of 760 °C for 686 MPa but weaken high temperature stress rupture properties. The (Al + Ta) content over 14.4 at.% led to the formation of large amounts of eutectic γ′ and exceeded the solubility of W and Mo in the residue liquid pool, which then promoted the precipitation of primary α-(W,Mo) and M₆C phases. Tantalum was also found as a strong MC carbides forming element. The order of ability to form monocarbide decreased from NbC to TaC to TiC. 6Al–0Ta (wt.%) alloys possessed good microstructural stability with no harmful topologically close-packed (TCP) phases being observed after thermal exposure at 850 °C/3000 h, 900 °C/1000 h. Only trace amounts of secondary plate-like M₆C carbides appeared in Ta-free and 5Al–4Ta (wt.%) alloys at 1100 °C/100–500 h. However, excessive Ta addition will destabilize the alloy and large amounts of secondary plate-like M₆C carbides precipitated after thermal exposure at 1100 °C. The transmission electron microscopy (TEM) and selected area electron diffraction (SAED) results showed the existence of the plate-like M₆C carbides.     

Catalytic synthesis of long NbS2 nanowire strands

Large-scale of long NbS₂ nanowire strands were successfully synthesized by a catalyzed transport reaction involving C₆₀. The strands have a diameter of 1–2 μm and length up to 0.5 mm, which are composed of single nanowire. The diameter of single nanowire is 1.6–20 nm. The products were characterized by powder X-ray diffraction, transmission electron microscopy, selected area electron diffraction, high-resolution transmission electron microscopy, scanning electron microscopy, and X-ray photoelectron spectroscopy. Probable mechanisms for catalytic growth were proposed.     

Vapor phase growth of GaN crystals with different morphologies and orientations on graphite and sapphire substrates

GaN crystals were grown on graphite and sapphire substrates at 990–1050 °C by reaction of Ga₂O with flowing NH₃. Ga₂O gas was produced at a constant rate (1.3 wt% min⁻¹) by reaction of Ga₂O₃ with carbon at 1000–1060 °C. The effect of NH₃ concentration (3–100 vol%) and the nature of the substrate on the morphology and orientation of the GaN crystals were determined by scanning electron microscopy, transmission electron microscopy, X-ray diffraction and selected area electron diffraction. It was found that sheet and plate-like crystals grew at different orientations to the substrate with different NH₃ concentrations and substrates.     

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.     

Characterization and synthesis of KTa0.1Nb0.9O3 particles via high temperature mixing method under hydrothermal conditions

KTa_0.1Nb_0.9O₃ (KTN) particles with an orthorhombic perovskite structure have been synthesized via a high temperature mixing method (HTMM) under hydrothermal conditions. The obtained samples were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), transmission electron microscopy (TEM), selected area electron diffraction (SAED), and high-resolution transmission electron microcopy (HRTEM). The influence of alkaline concentration and solvent composition on the phase structure and morphology of the obtained powders was investigated. The results show that the well-crystallized KTN powders with sizes of 200–500 nm are successfully prepared at temperatures as low as 240 °C when the KOH concentration is 2.0 M and the isopropanol/water (I/W) volume ratio equals to 100/0.     

Polyaniline nanowire electrodes with high capacitance synthesized by a simple approach

Polyaniline (PANI) nanowire electrodes were successfully synthesized by electrodeposition using starch as template. The electrodes were characterized with scanning electron microscope (SEM) and X-ray diffraction technique. SEM images showed that the electrodes electrodeposited using the starch template had nanowire morphology, but the PANI electrodeposited in absent solution had agglomerate block morphology. Cyclic voltammograms at different scan rates and charge–discharge tests were performed in 0.5 M H₂SO₄ aqueous solution. The PANI nanowire electrodes had a high capacitance (882 F g^? 1) and a high stability (5% capacity loss after 500 cycles).     

Anionic surfactant-assisted hydrothermal synthesis of high-aspect-ratio ZnO nanowires and their photoluminescence property

ZnO nanowires with high-aspect-ratio of up to ca. 600 were synthesized in a quaternary reverse microemulsion containing sodium dodecyl sulfate (SDS) / water / heptane / n-hexane via a hydrothermal method. SDS, as an anionic surfactant, plays an important role in the formation of morphologies. Subsequently, we studied lots of key influencing factors including the molar ratio (w) value of NaOH to Zn(OAc)₂, the reaction temperature, and the instance without the quaternary reverse microemulsion. The selected-area electron diffraction (SAED) and high-resolution transmission electron microscopy (HRTEM) reveal the single-crystal nature of the ZnO nanowires. The morphologies and crystalline structure of the as-obtained products were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM) and powder X-ray diffraction (XRD), respectively. Through this route, we can obtain a mass of products and the method is both convenient and reproducible. Finally, we measured the photoluminescence (PL) spectra and found that the ZnO nanowires exhibited green-orange emission at 525 nm and short ultraviolet emission at 380 nm and the ZnO nanomaterials with different aspect ratio (length to diameter) (L / D) showed PL intensity disciplinary change. Aiming at this phenomenon, we propose a reasonable mechanism to explain the PL spectra of the ZnO nanomaterials in detail.     

Structural defects in PbMoO4 single crystals doped with Co2+ ions

Pure and Co-doped PbMoO₄ crystals, were studied using reflection high energy electron diffraction (RHEED), optical and dielectric methods. The calculated lattice constants for PbMoO₄:Co (0.2 mol%) were determined as being equal to: a = 5.54 ± 0.05 Å and c = 11.96 ± 0.05 Å. The absorption spectra of “as grown” and annealed pure and Co-doped PbMoO₄ crystals were examined. The results of dielectric measurements gave the conductivity activation energy of highly Co-doped PbMoO₄ crystals (0.5 and 1.0 mol%) equal to 0.40 and 0.46 eV, respectively.     

Comparative dielectric studies of nanostructured BaTiO3, CaCu3Ti4O12 and 0.5BaTiO3⋅ 0.5CaCu3Ti4O12 nano-composites synthesized by modified sol–gel and solid state methods

BaTiO₃ (BTO), CaCu₃Ti₄O₁₂ (CCTO) and 0.5BaTiO₃·0.5CaCu₃Ti₄O₁₂ (BTO–CCTO), as a new nano-composite ceramic, were successfully designed and fabricated by a semi-wet gel route and a modified solid state method. The dielectric properties of the BTO–CCTO ceramic were compared to those of the BTO and CCTO ceramics at lower sintering temperatures and durations. The X-ray diffraction analysis revealed that the BTO and CCTO ceramics form a single crystalline phase and the average crystalline sizes calculated from X-ray diffraction data were in the range of 40–65 nm. The particle sizes of the BTO, CCTO, and BTO–CCTO ceramics obtained from transmission electron microscopy images were in the ranges of 40–65 nm, 80–110 nm, and 70–95 nm, respectively. The phase composition and microstructure were studied by X-ray diffraction and scanning electron microscopy. The energy dispersive X-ray results demonstrated the purity and stoichiometry of the BTO–CCTO nano-composite. The grain sizes of the BTO, CCTO and BTO–CCTO ceramics were found to be in the ranges of 500 nm–1 μm, 4–24 μm, and 250 nm–4 μm, respectively. The AC conductivity as a function of frequency confirmed the semiconducting nature of all of the ceramics and obeyed the Jonscher's power law. The impedance spectrum measurement result showed that the CCTO ceramic possessed an exceptional grain boundary resistance, which supports the internal barrier layer capacitance (IBLC) mechanism present in this ceramic and is responsible for the high ε_r values.     

Environmentally friendly growth of single-crystalline K2Ti6O13 nanoribbons from KCl flux

Single-crystalline K₂Ti₆O₁₃ nanoribbons with typical width ranging from one hundred nanometers to a few hundred nanometers and length up to tens of microns were prepared from KCl flux. The nanoribbons were characterized by a range of methods including X-ray diffraction, scanning electron microscopy, transmission electron microscopy, energy dispersive X-ray spectroscopy, selected area electron diffraction and high-resolution transmission electron microscopy. Ultraviolet–visible experiments showed that the K₂Ti₆O₁₃ nanoribbons were wide-band semiconductors with a band width E_g = 3.4 eV. The mechanism of one-dimensional growth of the nanoribbons was attributed to the oriented attachment mechanism.