Thermal scanning studies of percolated Fe–Cu granular alloys

Fe–Cu alloys produced by mechanical alloying were studied with Mössbauer thermal scanning spectroscopy (MTS). This technique consists in recording Mössbauer effect absorption at a fixed energy while the temperature of the sample is changed. Hyperfine magnetic field behavior can be closely followed. Four mechanically alloyed samples Fe_xCu_100−x with iron concentration x=30, 35, 40, and 45 at.% were studied. Absorption graphs (intensity vs. temperature) are similar for all samples: intensity sharply falls with the increase of the temperature, following the collapse of the sextet lines. This collapse occurs at a very precise temperature, which coincides with a magnetic–nonmagnetic transition line in a former magnetic phase diagram. Conventional Mössbauer spectroscopy confirms the appointed phase change, displaying a doublet at temperatures above the critical.     

Interfacial reactions in aluminum alloys/mullite–zirconia composites

Mullite and reaction-sintered mullite–zirconia bars were exposed to Mg- and Mg+Cu-containing molten aluminum alloyS, at 800°C for up to 2000 h, and afterwards characterized by X-ray diffraction (XRD), reflected light optical microscopy (RLOM) and scanning electron microscopy (SEM) with energy dispersive spectroscopy (EDS). Mullite was completely attacked by Al penetrating through grain boundaries and reducing the mullite grains to alumina and silicon. Mullite–zirconia was not attacked, because the dense net of ZrO₂-grains prevented penetration of molten metal into the compact and, consequently, a mechanically and thermodynamically stable spinel layer (≈30 μm) was formed at the static interface, which protected the ceramic against further attack.     

Soft magnetic amorphous Fe–Zr–Si(Cu) boron-free alloys

Amorphous Fe₈₀Zr_xSi_20−x−yCu_y boron-free alloys, in which boron was completely replaced by silicon as a glass forming element, have been prepared in the form of ribbons by using the melt quenching technique. X-ray diffraction and Mössbauer spectroscopy measurements revealed that the as-quenched ribbons with the compositions with x = 6–10 at.% and y = 0, 1 at.% are fully or predominantly amorphous. Differential scanning calorimetry (DSC) measurements allowed the estimation of crystallization temperatures of the amorphous alloys. Soft magnetic properties have been studied by the specialized rf-Mössbauer technique. Since the rf-collapse effect observed is very sensitive to the local anisotropy fields it was possible to evaluate the soft magnetic properties of the amorphous alloys studied. The rf-Mössbauer studies were accompanied by conventional measurements of hysteresis loops from which the magnetization and coercive fields were estimated. It was found that amorphous Fe–Zr–Si(Cu) alloys are magnetically very soft, comparable with those of the conventional amorphous B-containing Fe-based alloys.     

Interfacial properties of immiscible Co–Cu alloys

Using electromagnetic levitation under microgravity conditions, the interfacial properties of an Cu₇₅Co₂₅ alloy have been investigated in the liquid phase. This alloy exhibits a metastable liquid miscibility gap and can be prepared and levitated in a configuration consisting of a liquid cobalt-rich core surrounded by a liquid copper-rich shell. Exciting drop oscillations and analysing the frequency spectrum, both surface and (liquid–liquid) interfacial tension can be derived from the observed oscillation frequencies. This paper briefly reviews the theoretical background and reports on a recent experiment carried out on board the TEXUS 44 sounding rocket.     

Interfacial reactions in Sn–20In–2.8Ag/Cu couples

Interfacial reactions between Sn–20 wt.%In–2.8 wt.%Ag (Sn–20In–2.8Ag) Pb-free solder and Cu substrate at 250, 150, and 100 °C were investigated. A scallop-type η-Cu₆Sn₅ phase layer and a planar ε-Cu₃Sn phase layer formed at the interface at 250 °C. The indium content in the molten solder near the interface was increased with the formation of the η-Cu₆Sn₅ phase; and the η-Cu₆Sn₅, Ag₂In, Cu₂In₃Sn, and γ-InSn₄ phases formed from the solidification of the remaining solder. At 100 and 150 °C, only the η-Cu₆Sn₅ phase was found at the interface. However, unusual liquid/solid reaction-like interfacial morphologies, such as irregular elongated intermetallic layers and isolated intermetallic grains, were observed in the solid-state reactions. These η phase layers had less Sn content than the Sn–20In–2.8Ag alloy, resulting in an excess Sn-rich γ-InSn₄ phase accumulating at the interface and forming porous η layers on top of the initially formed dense η layers at 150 °C. At 100 °C, large elongated η grains were formed, whereas the interfacial layers remained almost unchanged after prolonged reaction. Based on the experimental evidence, the growth of the η phase was proposed to follow a diffusion-controlled mechanism at 250, 150 and 100 °C, while that of the ε phase was probably controlled by the reaction.     

Bioactive magnetic nanoparticles of Fe–Ga synthesized by sol–gel for their potential use in hyperthermia treatment

Hyperthermia is one of the most recents therapies for cancer treatment using particles with nanometric size and appropriate magnetic properties for destroying cancer cells. Magnetic nanoparticles (MNP’s) of Fe–Ga and synthesized using a polycondensation reaction by sol–gel method were obtained. MNP’s of Fe_1.4Ga_1.6O₄ that posses an inverse spinel structure were identified by X-Ray Diffraction, Transmission Electron Microscopy, Scanning Electron Microscopy and Energy Dispersive Spectroscopy. The results showed that the MNP’s are composed only by Fe, Ga and O and their size is between 15 and 20 nm. The magnetic properties measured by Vibration Sample Magnetometry demonstrated a saturation magnetization value of 37.5 emu/g. To induce the MNP’s bioactivity, a biomimetic method was used which consisted in the immersion of MNP’s in a Simulated Body Fluid (SBF) for different periods of time (7, 14 and 21d) along with a wollastonite disk. The formation of a bioactive layer, which closely resembles that formed on the existing bioactive systems and with a Ca/P atomic ratio within a range of 1.37–1.73 was observed on the MNP’s. Cytotoxicity of MNP’s was evaluated by in vitro hemolysis testing using human red blood cells at concentrations between 0.25 and 6.0 mg/mL. It was found that the MNP’s were not cytotoxic at none of the concentrations used. The results indicate that Fe–Ga MNP’s are potential materials for cancer treatment of both hard and soft tissue by hyperthermia and drug carriers, among other applications.     

Correlation of microstructure and magnetic properties in Cu–Co–Ni alloys

The present study concerns correlation of microstructure and magnetic properties of nanocrystalline binary 50Cu–50Co and ternary 50Cu–25Co–25Ni (wt%) alloys prepared by ball milling and subsequent isothermal annealing of the ball milled alloys. High resolution transmission electron microscopic (HR-TEM) investigation has shown deformation-induced microstructural features. Field emission scanning electron microscopy (FE-SEM) has revealed a distinct change in morphology of as-milled CuCoNi alloys after annealing. Differential scanning calorimetric (DSC) and X-ray diffraction (XRD) analysis have revealed that annealing of the CuCoNi alloy above 350 °C results into precipitation of nanocrystalline Co (fcc) in the CuNi matrix by spinodal decomposition. It is also demonstrated that isothermal annealing of the ball milled alloys in the temperature range between 350 and 650 °C significantly influence the magnetic properties, e.g. coercivity (H_c), remanence (M_r) and magnetic saturation (M_s) due to annihilation of defects such as stacking and twin fault along with dissolution and/or precipitation of magnetic phases in the Cu-rich matrix.     

Structure of metastable precipitate in some Al–Cu–Mg–Ag alloys

Abstract

The high strength of some Al–Cu–Mg–Ag alloys has been attributed to very thin (~2·5 nm), but broad, hexagonal-shaped precipitates. Previous work has shown that the precipitates have a hexagonal unit cell, but different lattice parameters have been reported. In the present paper, the intensities of X-ray diffraction reflections from the precipitates have been measured on Buerger precession photographs, and it is shown that the crystal structure is monoclinic (space group P2/m) with the parameters a = b = 0·496 nm, c = 0·848 nm, γ = 120°. The special values of these parameters confer a hexagonal symmetry on the lattice. This unusual structure is a slightly distorted form of θ-CuAl₂, to which it appears to change after long aging times at 200°C.     

Microwave absorption performance of magnetic Fe–Ni–P nanoparticles electrolessly plated on hollow glass microspheres

Magnetic Fe–Ni–P nanoparticles have been successfully fabricated on hollow glass microspheres via electroless plating for the application of lightweight microwave absorbers. The resultant materials were characterized by field emission-scanning electron microscopy (FE-SEM), energy dispersive X-ray (EDX), X-ray diffraction analysis (XRD), vibrating sample magnetometer (VSM) and vector network analyzer. The results show that compact and uniform Fe–Ni–P nanoparticles with the average diameter of about 150 nm have been successfully plated on the hollow glass microspheres. The plated microspheres exhibit excellent soft magnetic characteristics with high saturation magnetization and low coercivity, and the soft magnetic characteristic behaves better with the increasing of iron content in the coatings. Microwave absorption performance shows the maximum reflection loss of the composite powder reaches −49.2 dB at the frequency of 7.7 GHz with the thickness of 5 mm, and the bandwidth with the reflection loss less than −20 dB exceeds 2.2 GHz.     

Alloying element nitride stability in iron-based alloys; denitriding of nitrided Fe–V alloys

Recognising the various types of absorbed nitrogen in nitrided iron-based alloys and the lack of accuracy in local composition analysis of the individual nano-sized nitride precipitates (e.g. by atom probe tomography), precise determination of the nitride composition requires so-called denitriding treatments. This study proposes two routes to determine the nanonitride stoichiometry, which are demonstrated by experimental analysis of the denitriding behaviour in hydrogen gas of nitrided, model Fe–V alloys. The minimal nitrogen activity to stabilise the alloying element nitrides MeN in Fe–Me–N alloys is calculated. A strategy is offered to stabilise the alloying element nitrides and to determine the nitrogen content strongly bonded in the nitrides.     

Positron annihilation study on deformation-induced Au precipitation in Fe–Au and Fe–Au–B–N alloys

We have investigated the potential self-healing of deformation-induced defects by Au precipitation during isothermal aging at 550 °C in Fe–Au and Fe–Au–B–N alloys using positron annihilation spectroscopy. Two different samples with 0 and 24 % pre-strain were used to study the influence of dislocations on the Au precipitation. Dislocations introduced prior to the aging process play an essential role in the formation of Au precipitates. The Coincidence Doppler broadening (CDB) technique shows that Au precipitation in the matrix occurs in the pre-strained samples only. TEM observations confirm the heterogeneous nature of the Au precipitation which occurs exclusively on dislocations and grain boundaries. The evolution of S and W parameters derived from the CDB indicates a three-stage precipitation process for the pre-strained samples. Both the hardness tests and the positron annihilation spectroscopy indicate that the addition of boron and nitrogen to the Fe–Au alloy causes a deceleration of the Au precipitation in the pre-strained samples, but does not alter the defect-induced mechanism of the Au precipitation. The defect-induced Au precipitation provides a promising site-specific autonomous repair mechanism to extend the lifetime of Fe-based alloys for high temperature structural applications.     

The detection of a strong influence of composition variations on low-temperature magnetic ordering in nearly stoichiometric Fe–V–Al alloys

The magnetic state of Fe–V–Al alloys with nearly stoichiometric (Fe₂VAl) compositions varying with respect both to aluminum and transition elements was studied. The effect of strong qualitative change in the magnetic properties induced by small variations of the composition was observed for the first time and analyzed. The key result is the detection of ferromagnetic ordering with a relatively high (~50 K) Curie temperature in an alloy with V atoms substituted in the lattice by Al atoms and the Fe content corresponding to the stoichiometric composition.     

Anelasticity of Fe–Ga based alloys

Frequency, amplitude, and temperature dependent effects of anelasticity in Fe–Ga and Fe–Ga–Al alloys are studied by mechanical spectroscopy techniques using forced bending and torsion subresonance vibrations (f from 0.001 to 200 Hz, ε from 10^− 6 to 10^− 2, T from 0 to 600 °C). The structure and the properties of the studied alloys are characterized by scanning electron microscopy and magnetic force microscopy. Main regularities of amplitude dependent damping are attributed to magnetomechanical damping, which is very sensitive to the structural state of alloys, their composition, magnetostriction, and testing method. Two maximal damping peaks at about 18% and 27%Ga correspond to similar maxima of magnetostriction against %Ga. Both temperature dependent thermally activated relaxation effects and anelastic effects due to phase transitions are discussed in terms of alloys structures. Thermally activated internal friction peaks are ascribed to different atomic mechanisms. A phase transition from bcc originated structures (A2 and D0₃) to an fcc ordered structure (L1₂) is accompanied by a transient anelastic effect typical for a shear diffusionless transition.     

Precipitation behavior of Ag–Pd–In dental alloys

Age-hardening characteristics and precipitation behavior of Ag–25%Pd–3%In–1%Zn–0.5%Ir alloy were investigated in detail by means of hardness testing, X-ray diffraction, electron microscopy and resistivity measurement. The solution treating could be accomplished at 980 °C and the aging in the temperature range from 950 to 850 °C occurred by continuous precipitation. The aging in the temperature range from 850 to 450 °C occurred first, forming GP-zones with a hardness increase and then in overaging stage by forming discontinuous precipitation, which consisted of lamellae of solute (Pd, In, Zn) depleted Ag-rich phase and (Pd,Ag)₃(In,Zn) intermetallic phase. The hardness increased very fast to its peak in 10 min during aging at temperatures between 450 and 550 °C.     

Solidification microstructures selection of Fe–Cr–Ni and Fe–Ni alloys

The transition of solidified phases in Fe–Cr–Ni and Fe–Ni alloys was investigated from low to high growth rate ranges using a Bridgman type furnace, laser resolidification and casting into a substrate from superheated or undercooled melt. The ferrite–austenite regular eutectic growth, which is difficult to find in typical production conditions of stainless steels, was confirmed under low growth rate conditions. The transition velocity between eutectic and ferrite cell growth had a good agreement predicted by the phase selection criterion. Which of either ferrite or austenite is easier to form in the high growth range was discussed from the point of nucleation and growth. Metastable austenite formation in stable primary ferrite composition was mainly a result of growth competition between ferrite and austenite. For a binary Fe–Ni system, a planar metastable austenite in the steady state, simultaneous growth such as eutectic and banded growth between ferrite and austenite in an initial transient region are confirmed.     

Phase transformations in Fe–Ni–Cr heat-resistant alloys for reformer tube applications

Fe–35Ni–25Cr–0.4C alloys with different compositions are aged between 750 and 1150°C up to ～10,000?h. As-cast microstructure contains interdendritic carbides of type M₇C₃ (‘Cr₇C₃’) and MC (‘NbC’). At service temperatures, M₇C₃ transform into M₂₃C₆ (‘Cr₂₃C₆’) within hours. Then, a hardening precipitation of secondary intragranular M₂₃C₆ occurs over hundreds of hours, the nose of the ‘temperature-time-hardening’ curve being around 1000°C. G phase forms after long aging; its solvus temperature and formation kinetics depend on silicon content. Z phase is observed after long aging at 950°C or above. G and Z phases form at the expense of MC. Very long aging causes nitridation under air, with first a transformation of M₂₃C₆ into chromium-rich M₂X carbonitrides (X?=?C,N), then of MC into chromium-rich MX carbonitrides.     

Liquid-state and solid-state interfacial reactions between Sn–Ag–Cu–Fe composite solders and Cu substrate

The growth kinetics and morphology of the interfacial intermetallic compound (IMC) between Sn–3Ag–0.5Cu–xFe (x = 0, 0.5 wt%, 1 wt%) composite solders and Cu substrate were investigated in the present work. The Sn–Ag–Cu–Fe/Cu solder joint were prepared by reflowing for various durations at 250 °C and then aged at 150 °C. During soldering process, Fe particles quickly deposited in the vicinity of IMC, resulting in the formation of Fe-rich area. Isothermal equation of chemical reaction and phase diagrams were used to explain the effect of Fe on the growth kinetics of IMC during liquid-state interfacial reaction. It was shown that Fe could effectively retard the growth of interfacial Cu₆Sn₅ and Cu₃Sn layers during liquid-state reaction and reduce the size of Cu₆Sn₅ grains. Small cracks were observed in the Cu₆Sn₅ grains after reflowing for 2 min while they were found in the other composite solders reflowing for about 30 min. The Fe tended to suppress the growth of the Cu₃Sn layer during solid-state aging. However, the total thickness of IMCs (Cu₆Sn₅ + Cu₃Sn) for the composite solders with Fe particles was similar to that for SnAgCu without Fe particles.