Formation, properties and microstructure of amorphous/crystalline composite Ag20Cu30Ti50 alloy using miscibility gap

The aim of the work was to produce the amorphous/crystalline composite with uniform distribution of fine crystalline soft phase. Silver–copper–titanium Ag₂₀Cu₃₀Ti₅₀ alloy was prepared using 99.95 wt% Ag, 99.95 wt% Cu, 99.95 wt% Ti that were arc-melted in argon atmosphere. Then the alloy was melt spun on a copper wheel with linear velocity of 33 m/s. Investigation of the microstructure for both arc-melt massive sample and melt-spun ribbons was performed with use of scanning electron microscope (SEM) with EDS, light microscope (LM) and X-ray diffraction. The thermal stability was evaluated by differential scanning calorimetry (DSC). The properties such as Young modulus and Vickers hardness number before and after crystallization of the amorphous matrix were measured with use of nanoindenter. The microstructure was investigated by transmission electron microscope (TEM). It was found, that the alloy has a tendency for separation within the liquid state due to the miscibility gap which resulted in segregation into Ti–Cu–Ag matrix and Ag-base spherical particles after arc-melting. During rapid cooling through the melt spinning the Ag₂₀Cu₃₀Ti₅₀ alloy formed an amorphous/crystalline composite of fcc silver-rich spherical particles within the amorphous Ti–Cu–Ag matrix.     

Surface modification of Zr-based bulk amorphous alloys by using ion irradiation

Surfaces of the [Zr_0.65Cu_0.18Ni_0.09Al_0.08]₉₈M₂ (M = Er and Gd) bulk amorphous alloys were modified by irradiation with energetic singly charged argon (Ar⁺) ions. Samples of both the alloys were irradiated with 2.17 × 10¹⁷ argon ions of 10 keV energy. As cast and ion irradiated samples were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS). Mechanical properties like Vicker's hardness, nanohardness, elastic modulus and elastic recovery were measured. Considerable increase in elastic modulus and hardness was observed because of ion irradiation in these alloys. The ion irradiated samples of the [Zr_0.65Cu_0.18Ni_0.09Al_0.08]₉₈Er₂ alloy showed better properties as compared to [Zr_0.65Cu_0.18Ni_0.09Al_0.08]₉₈Gd₂ alloy. CuZr₂ phase was detected in ion irradiated alloys by XRD and confirmed by EDS. The range of Ar⁺ ions was found to be approximately 9.3 ± 5.4 nm in both alloys.     

Experimental study of phase transformations in 3003 aluminium alloys during heating by in situ high energy X-ray synchrotron radiation

This paper aims to study microstructural evolutions in the 3003 aluminium alloys during the heating part of the homogenization treatment from the as-cast state. After solidification, both the solid solution and primary precipitates are far from equilibrium. During a subsequent heating, an eutectoid transformation of the primary eutectic particles and a fine precipitation of dispersoids occur. The evolution of the precipitation amounts are obtained by high energy synchrotron radiation diffraction and microstructural observations (TEM and SEM) combined with image analysis. The analysis of these different results lead to the volume fraction evolutions of dispersoids and primary particles with temperature. Moreover, the different evolutions are compared to in situ electrical resistivity leading to propose the main causes of the variations observed.     

Influence of fluxing in the preparation of bulk Fe-based glassy alloys

Fe-based master ingots, with composition [(Fe₅₀Co₅₀)₇₅B₂₀Si₅]₉₆Nb₄, have been prepared by arc-melting and subsequently purified using the fluxing technique. Rods, with diameters from 1 to 2.5 mm, ribbons and wires with a maximal diameter of 200 μm have been produced from these purified master ingots. The amorphous structure, thermal stability, hardness and magnetic properties of the specimens were studied. In particular, we show by high-energy synchrotron X-ray diffraction that the rods are fully amorphous up to a maximal diameter of 2 mm. Moreover, the [(Fe₅₀Co₅₀)₇₅B₂₀Si₅]₉₆Nb₄ glassy alloy exhibits high hardness (HV = 1050) combined with good soft-magnetic properties (H_c = 63 A/m).     

Oxidation behavior of amorphous and nanoquasicrystalline Zr–Pd and Zr–Pt alloys

Oxidation behavior of amorphous and nanoquasicrystalline Zr₇₀Pd₃₀ and Zr₈₀Pt₂₀ alloys melt-spun at different wheel speeds has been studied in air by non-isothermal and isothermal techniques. Oxidation resistance of amorphous alloys has been found to be the lowest in comparison to the partially and fully crystallized Zr alloys. It has also been observed that oxidation does not induce crystallization of the amorphous phase. It has been shown that the oxygen diffusion rate increases gradually in the order of crystalline, nanoquasicrystalline, partially nanocrystalline and amorphous states of these alloys. Possible micromechanism of oxidation and the role of different grain/interface boundaries on the oxygen diffusion has been discussed.     

On the amorphous and nanocrystalline Zr–Cu and Zr–Ti co-sputtered thin films

In the current study, we examined and compared the mixing and vitrification behavior of the Zr–Cu and Zr–Ti binary systems in the form of co-sputtered thin films with or without post-annealing. The co-sputtered Zr–Cu films are all amorphous under various co-sputtering conditions, suggesting the high vitrification tendency. The amorphous Zr–Cu thin film will start to crystallize into nano-crystalline Zr₂Cu and Zr₇Cu₁₀ phases upon long exposure at temperatures above 350 °C. On the other hand, it is difficult to form amorphous film with the Zr–Ti system, except at a low sputtering power of 30–50 W. The low powers enable the co-sputtered Zr–Ti thin film to exhibit the diffuse hump in the X-ray diffraction. Examination by high resolution transmission electron microscopy reveals numerous fine nano-crystalline phases around 2 nm in the amorphous matrix. Upon exposure at 700 °C, the Zr–Ti films transform into crystalline hexagonal close-packed α and body-centered cubic β phases.     

Temperature-dependant non-catalytic growth of ultraviolet-emitting ZnO nanostructures on silicon substrate by thermal evaporation process

Needle-like nanowires, nanorods, and nanosheets containing nanowires of ZnO have been synthesized on silicon substrate by the thermal evaporation of metallic zinc powder in the presence of oxygen without the use of any catalyst or additives. It was observed that a particular type of ZnO nanostructure can be obtained in a specific temperature zone and morphology can be well controlled simply by adjusting the substrate temperature. Detailed structural analysis revealed that the formed ZnO nanostructures are single-crystalline with wurtzite hexagonal phase, grown along the [0 0 0 1] direction in preference. Raman scattering and room-temperature photoluminescence spectra showed the good crystallinity with hexagonal wurtzite phase and excellent optical properties, respectively for all the deposited ZnO nanostructures.     

Synthesis and characterization of neodymium oxide nanoparticles

The nanometric precursors of neodymium oxide of various morphology from fibrous to well-dispersed spheroidal were prepared via a solvothermal reaction routes. The precursors and their thermal evolution to neodymium oxide phase were characterized by means of X-ray diffraction (XRD), transmission electron microscopy (TEM) and scanning electron microscopy (SEM). It was found that the reaction parameters, kind of solvent as well as neodymium salt used played a key role for the product formation of desired morphology and structure. Similarly, kind of neodymium oxide precursor determined the morphology and the crystal structure (haxagonal or cubic) of the final oxide. The potential application of Nd₂O₃ precursors prepared by solvothermal method as convenient material for preparation of homogeneous thin coatings on planar substrates is shown.     

Correlation between the synthesis conditions and the compositional and magnetic properties of Co2(Cr1−xFex)Al Heusler alloys

In this study we give evidence for the strong dependence of the compositional and magnetic properties on the synthesis conditions of polycrystalline Co₂(Cr_1−xFe_x)Al Heusler alloys (0 ≤ x ≤ 1) by comparing the properties of as-grown and annealed compounds. Strong chemical inhomogeneities are found at the micrometric level depending on the compound and the synthesis method. Moreover, we find that the Co content is homogeneous at the micrometric level in all the studied samples in sharp contrast with significant inhomogeneous distribution of (Fe/Cr) and Al at the micrometric level, especially for Cr-rich compounds (x ≤ 0.4). We have found that the magnetic properties (the Curie temperature and the saturation magnetization) are strongly depressed in the annealed compounds with respect to the corresponding as-grown compounds. For the as-grown compounds the saturation magnetization is close to the theoretically predicted one for x ≥ 0.7 whereas it is lower than the theoretically predicted one for x ≤ 0.4, which correlates with the observed chemical inhomogeneity.     

Reinforcement of Al–Fe–Ni alloys with the in situ formation of composite materials

One of the most effective methods for the improvement of the mechanical properties of metals is their reinforcement with non-metallic materials. In the present work powder of K₂TiF₆ and KBF₄ was added in an Al–Fe–Ni alloy while the alloy was in liquid form at 1060 °C with a 5 wt.% mixture of powders and with simultaneous stirring for 30 min. The liquid was squeeze-casted at 150 bar. The as-cast specimens were examined with electron microscopy and X-ray diffraction. SEM analysis revealed that the as-formed material is composed by needle-like crystallites along with a dentritic form and an interdendritic phase. The composition of the needle-like crystallites may presumably be expressed by the formula (Fe-Ni)Al₃. The rest of the matrix consists of almost pure Al grown dentritically, while the interdendritic phase contains Fe and Ni dissolved in Al. EDS analysis also proved the existence of spots with high Ti concentration, which probably refer to the Ti–B compounds. Finally TEM verified the presence of nanocrystals in the matrix.     

Amorphous and nanocrystalline sputtered Mg–Cu thin films

Binary Mg–Cu amorphous alloys were first fabricated in 1980s via liquid quenching. In this study, the Mg_1−xCu_x (x varying from 38 at.% to 82 at.%) partially amorphous thin films are prepared via co-sputtering. Upon thermal annealing, the Mg₂Cu or MgCu₂ nanocrystalline phases are induced in the Mg-rich or Cu-rich thin films, respectively. Due to the presence of fine nanocrystalline Mg₂Cu or MgCu₂ particles in the Mg–Cu amorphous matrix, the as-sputtered thin films show satisfactory Young's modulus 100 GPa and hardness 4 GPa.     

Structural study on Zr0.39Ni0.61 and (Zr0.39Ni0.61)D0.59 amorphous alloys by neutron and X-ray diffraction

Neutron and X-ray diffraction and reverse Monte Carlo (RMC) simulation were performed on Zr_0.39Ni_0.61 and (Zr_0.39Ni_0.61)D_0.59 amorphous alloys to investigate the rearrangement of metal atoms due to the deuterium absorption. The RMC models showed that the Zr–Zr distances slightly increase but the Zr–Ni and Ni–Ni distances remain virtually unchanged after the deuterium absorption. Additionally, the Voronoi polyhedral analysis of the RMC configurations showed that there is not much difference in the local structure around Zr and Ni between Zr_0.39Ni_0.61 and (Zr_0.39Ni_0.61)D_0.59 amorphous alloys.     

Effect of the addition of In on the microstructural formation of Sn–Ag–Zn lead-free solder

The effect of addition of In, up to 1 wt.%, on the formation of intermetallic compounds (IMCs) in the solidified Sn–3.7%Ag–0.9%Zn lead-free solder was investigated. As observed by microstructural analysis, the typical structure of Sn–Ag–Zn solder is composed of β-Sn phase and mixed granules of Ag₃Sn and AgZn IMCs. After alloying with In, it evolves into a mixture of randomly distributed rods and granules of Ag₃Sn and AgZn. Clearly, the addition of In into the explored Sn–Ag–Zn solder promotes the formation of rod-like IMCs for the reason that the growth competition of the Ag₃Sn and AgZn IMCs was destroyed by the selective adsorption of In atoms on a certain preferable crystalline planes of the separated IMCs. The change in the morphology of the formed IMCs leads to a great difference in the mechanical performances, for example, the measured microhardness of the investigated solders evolves from 16.95 HV to 21.35 HV with the increase of In content.     

Synthesis of (Ti,W, Mo,V)(C,N) nanocomposite powder from novel precursors

(Ti, W, Mo, V)(C, N) nanocomposite powders with globular-like particle of ∼10–100 nm were synthesized by a novel method, namely carbothermal reduction–nitridation (CRN) of complex oxide–carbon mixture, which was made initially from salt solution containing titanium, tungsten, molybdenum, vanadium and carbon elements by air drying and subsequent calcining at 300 °C for 0.5 h. Phase composition of reaction products was discussed by X-ray diffraction (XRD), and microstructure of the calcined powders and final products was studied by scanning electron microscopy (SEM) and transmission electron microscope (TEM), respectively. The results show that the synthesizing temperature of (Ti, W, Mo, V)(C, N) powders was reduced greatly by the novel precursor method. Thus, the preparation of (Ti, 15W, 5Mo, 0.2V)(C, N) is at only 1200 °C for 2 h. The lowering of synthesizing temperature is mainly due to the homogeneous chemical composition of the complex oxide–carbon mixture and its unusual honeycombed structure.     

A simple catalyst-free route for large-scale synthesis of SiC nanowires

A large number of SiC nanowires were fabricated by a simple catalyst-free method using silicon powders and expandable graphite as raw materials. Digital camera, X-ray diffractometer, Fourier transform infrared spectrometer, field-emission scanning electron microscopy and transmission electron microscopy demonstrate that a large number of loose products were obtained in graphite crucible. The products are composed of single crystalline 3C-SiC nanowires with lengths up to several tens of micrometers and diameters of 20-60 nm. The vapor-solid mechanism was proposed to interpret the growth procedure of SiC nanowires. The expandable graphite as carbon source can provide enough growth space for nanowires, which is helpful to improve the yield of SiC nanowires. The simple method provides a promising candidate for industrial fabrication of SiC nanowires.     

Improvement of the magnetic properties of nanocomposite permanent magnetic alloys with Dy and Ga substitutions

The Dy and Ga substituted NdFeB nanocomposite permanent magnetic alloys with high magnetic properties have been prepared by appropriate wheel speed of melt-spinning and post-annealing treatment. Under optimal conditions, compared with the best magnetic properties of ternary NdFeB alloy of J_r=1.18 T, H_ci=379.5 kA/m and (BH)_max=119.5 kJ/m³, the best magnetic properties of the alloy with Dy and Ga substitutions are J_r=1.16 T, H_ci=580.5 kA/m, and (BH)_max=162.7 kJ/m³. The XRD and TEM results showed that each of two alloys consists of hard magnetic 2:14:1 phase and soft magnetic α-Fe phase. The grain size of the 2:14:1 phase is about equal in the two alloys. The grain size and content of α-Fe phase in Dy and Ga substituted alloy are finer and lower, respectively.     

Glycolthermal synthesis and characterization of hexagonal CdS round microparticles in flower-like clusters

Hexagonal CdS round microparticles in flower-like clusters were synthesized by glycolthermal reactions of CdCl₂ and thiourea as cadmium and sulphur sources in 1,2-propylene glycol (PG) at 100-200 °C for 10-30 h. Phase and morphology were detected using X-ray diffraction (XRD), and scanning and transmission electron microscopy (SEM, TEM). The products were pure phase of hexagonal wurtzite CdS. The quantitative elemental analysis of Cd:S ratio was detected using energy dispersive X-ray (EDX) analyzer. Raman spectrometer revealed the presence of fundamental and overtone modes at 296 and 595 cm⁻¹, corresponding to the strong 1LO and weak 2LO modes, respectively. Photonic properties were investigated using UV-visible and photoluminescence (PL) spectroscopy. They showed the same absorption at 493-498 nm, and emission at 431 nm due to the excitonic recombination process. A possible formation mechanism was also proposed, according to experimental results.     

Small-angle subgrain boundaries emanating from dislocation pile-ups in multicrystalline silicon studied with synchrotron white-beam X-ray topography

The formation of dislocation pile-ups and related small-angle subgrain boundaries in block-cast multicrystalline silicon for photovoltaic applications has been studied by means of white-beam X-ray topography (WB-XRT). For this purpose, samples sliced perpendicular and parallel to the growth direction have been investigated in reflection and transmission geometry, respectively. During the growth process of the silicon ingot, the dislocation density increases. WB-XRT measurements revealed the formation of small-angle subgrain boundaries. The subgrains have a slightly changed orientation related to a rotation of ～0.07–0.80° around an axis parallel to the growth direction. This tilt results from the high number of dislocations forming dislocation pile-ups and walls. The spacings between dislocations in such subgrain boundaries were found to be between 297 and 28 nm. A qualitative model for the formation of dislocation pile-ups is proposed.     

Novel Al-matrix nanocomposites reinforced with multi-walled carbon nanotubes

Novel Al-based nanocomposites reinforced with multi-walled carbon nanotubes were produced by mechanical milling followed by pressure-less sintering at 823 K under vacuum. The interface between Al matrix and the multi-walled carbon nanotubes was examined using transmission electron microscopy. These observation showed that the multi-walled carbon nanotubes were not damaged during the preparation of the nanocomposite and that no reaction products were detected after sintering. The mechanical properties of sintered nanocomposites specimens were evaluated by a compression test. The yield stress (σ_y) and the maximum strength (σ_max) obtained were considerably higher than those reported in the literature for pure Al prepared by the same route. The values for σ_y and σ_max increase as the volume fraction of multi-walled carbon nanotubes increases. The milling time and the concentration of multi-walled carbon nanotubes have an important effect on the mechanical properties of the nanocomposite.