Tetragonal phase in the Mg–Ni–Sn system

Complementary metallographic and crystallographic characterisations of the Mg-rich corner of the Mg–Ni–Sn system are presented. In particular the Mg₇₅Ni₁₅Sn₁₀ phase, previously reported by Arcondo et al. [Hyperfine Interact. 66 (1991) 359] has been identified as a tetragonal phase by transmission electron microscopy and X-ray diffraction studies. The influence of this new phase, called Y-phase, on the glass forming ability of alloys with nearby composition is discussed.     

Levels of thermal stability in some glassy alloys of the Ge–Sb–Se system by differential scanning calorimetry

The thermal stability and crystallization of alloys in the Ge–Sb–Se system were studied by differential scanning calorimetry (DSC). A comparison of various simple quantitative methods to assess the level of stability of the glassy materials in the above-mentioned system is presented. All of these methods are based on characteristic temperatures, obtained by heating of the samples in non-isothermal regime, such as the glass transition temperature, T_g, the temperature at which crystallization begins, T_in, the temperature corresponding to the maximum crystallization rate, T_p, or the melting temperature, T_m. In this work, a parameter K_r(T) is added to the stability criteria. The thermal stability of some ternary compounds of Ge_xSb_0.23−ySe_0.77−x+y type has been evaluated experimentally and correlated with the activation energies of crystallization by this kinetic criterion and compared with those evaluated by other criteria.     

Preparation and structures of the La1−xKxCo1−xNbxO3 (x = 0–l) system

The La_1−xK_xCo_1−xNb_xO₃ system was performed by conventional solid state reaction technique using metal oxides. By DSC analysis, the activation energy of crystallization of the powders with x = 0.3 is 388.4 kJ/mol. The crystal structure of the compound reveals a transition from rhombohedral to cubic, and then to orthorhombic structure as the amount of the potassium niobate (KNbO₃) increases. It is found that the structure of the samples with x < 0.3 is similar to that of lanthanum cobaltate (LaCoO₃), while at the compositions with 0.7 ≥ x ≥ 0.3, the structure transforms to cubic. Finally, with x ≥ 0.7, the structures were similar to that of KNbO₃. According to the results of selected-area-diffraction (SAD) patterns and X-ray diffraction (XRD) identifications, the lattice parameters were calculated. The direction of superlattice structure along [2 1 0] was found for x = 0.5 as identified from SAD patterns. The dielectric constants were measured with cubic structure. Dielectric constant (K) decreases with increasing x.     

Solidification study of Al–Co–Cu alloys using the Bridgman method

The solidification of a series of Bridgman-grown Al–Co–Cu alloys with compositions in the vicinity of the quasicrystal was studied by powder X-ray diffraction (XRD), differential thermal analysis (DTA), electron microprobe analysis, and optical microscopy. The phase equilibria and microstructure of solidified alloys are presented; the temperatures of the involved solidification reactions were determined. These experimental data were used to construct a solidification phase diagram as to understand the crystallization path. The decagonal (D) AlCoCu quasicrystals form incongruently, but they can be primarily solidified from off-stoichiometric melts.     

La–Mg–Ni ternary hydrogen storage alloys with Ce2Ni7-type and Gd2Co7-type structure as negative electrodes for Ni/Mh batteries

Hydrogen strorage alloys with formula La_1.5Mg_0.5Ni₇ were prepared by induction melting followed by different annealing treatments (1073, 1123 and 1173 K) for 24 h. The alloy composition, alloy microstructure and electrochemical properties were investigated, respectively. The results showed that the multi-phase structure of as-cast alloy was converted into a double-phase structure (Gd₂Co₇-type phase and Ce₂Ni₇-type phase) through annealing treatments. Mg atoms were mainly located in Laves unit of Gd₂Co₇-type unit cell and Ce₂Ni₇-type unit cell. The electrochemical capacity of alloy electrodes after annealing treatment could be up to 390 mAh/g. The cyclic stability of alloy electrodes was significantly improved by annealing treatments; After 150 charge/discharge cycles, the capacity retention ratio of alloy annealed at 1173 K was the highest (81.9%). The high rate dischargeability of alloy electrodes was also improved due to annealing treatment.     

In situ XRD studies on Al–Ni and Al–Ni–Sr alloys prepared by rapid solidification

In this paper the structure and stability of Al–17 wt.%Ni(Al–17Ni) and Al–17 wt.%Ni–2 wt.%Sr alloys prepared by rapid solidification was investigated by means of XRD techniques. Our work demonstrates that both alloys are crystalline and composed of fcc (Al–Ni) solid solution and orthorhombic Al₃Ni phases. The ternary alloy shows in addition the presence of small amount of tetragonal Al₄Sr phase. In situ XRD experiment demonstrates the stability of the solute solution up to 650 °C, Al₃Ni above 750 °C while Al₄Sr overcomes melting of the major phases at 800 °C. High-temperature structure analysis proved strong bindings between Al and Ni atoms in Al₃Ni phase, corroborating its covalent nature, linear and faster increase of the fcc volume with annealing temperature. The linear correlation between constituting atoms decreases with increase of the temperature.The work also documents the applicability of pair distribution function (PDF) analysis to the study of multiphase crystalline systems.     

The isothermal section of the Gd–Ni–V ternary system at 773 K

The phase equilibria of the Gd–Ni–V system at 773 K were investigated by means of X-ray diffraction (XRD), scanning electron microscopy (SEM), and electron probe microanalysis (EPMA). The experimental results show no existence of ternary compounds at 773 K. The existence of 14 single-phase regions, 25 two-phase regions and 12 three-phase regions was determined. The maximum solubility of V in (Ni), Gd₂Ni₁₇, GdNi₅ and GdNi₂ was measured to be about 16 at.%, 2 at.%, 3 at.% and 2.5 at.%, respectively, while that of Gd in (Ni), Ni₃V, Ni₂V, Ni₂V₃, NiV₃ and (V) was less than 1 at.%. An isothermal section of the Gd–Ni–V system at 773 K has been presented according to the present work.     

Observation of hydrogen absorption/desorption reaction processes in Li–Mg–N–H system by in-situ X-ray diffractmetry

The in-situ XRD measurements on dehydrogenation/rehydrogenation of the Li–Mg–N–H system were performed in this work. The ballmilled mixture of 8LiH and 3Mg(NH₂)₂ as a hydrogenated phase gradually changed into Li₂NH as a dehydrogenated phase during heat-treatment at 200 °C in vacuum for 50 h. Neither Mg-related phases nor other intermediate phases were recognized in the dehydrogenated phase. With respect to the hydrogenation process, the dehydrogenated state gradually returned to the mixed phase of the LiH and Mg(NH₂)₂ without appearance of any intermediate phases during heat treatment at 200 °C under 5 MPa H₂ for 37 h and during slow cooling down to room temperature through 24 h. In the hydrogenation process at 200 °C under 1 MPa H₂, however, the growing up of the LiNH₂ and LiH phase was observed in the XRD profiles before the 3Mg(NH₂)₂ and 8LiH phases were formed as the final hydrogenated state. This indicates that the LiNH₂ and LiH phase essentially appears as an intermediate state in the Li–Mg–N–H system composed of 3Mg(NH₂)₂ and 8LiH.     

Effects of C particle size on the ignition and combustion characteristics of the SHS reaction in the 20 wt.% Ni–Ti–C system

C particle size plays an important role in the ignition and combustion characteristics of the SHS reaction in the 20 wt.% Ni–Ti–C system. When coarse C particles (38 and 75 μm) are used, the SHS reactions consist of two different combustion stages with different brightness intensity of the combustion wave; XRD results indicate that the first and second combustion stages mainly correspond to the formation of Ni–Ti compounds and TiC ceramics, respectively. However, the final reaction is incomplete with a few Ni–Ti compounds and unreacted C. In contrast, when the fine C particle (1 μm) is used, the SHS reaction consists of only one combustion stage with high brightness intensity of the combustion wave; XRD result indicates that final products consist of TiC and Ni, without any intermediate phase. With the decrease of C particle size, the wave velocities increase, and the ignition time becomes shorter. In addition, the morphology of TiC particulate changes to near-spherical, as C particle size decreases.     

Features of the HDDR process in R–Fe–B ferromagnetic alloys (R is a mixture of Nd, Pr, Ce, La, Dy and others)

Features of the conventional hydrogenation, disproportionation, desorption, recombination (HDDR) and solid-HDDR processes in some R–Fe–B (R is a mixture of Nd, Pr, Ce, La, Dy) ferromagnetic alloys were studied in the temperature range 20–990 °C and pressure range from 1×10⁻³ Pa to 0.1 MPa. This was carried out by means of differential thermal analysis (DTA), X-ray diffraction (XRD) analysis and scanning electron microscopy (SEM) methods. The hydride of the initial phase is formed by heating to 115 °C. The disproportionation of the alloys occurs in the temperature range from 320 to 800 °C. Φ-phase constitutes the base of the initial alloys. Among the disproportionation products, R-hydride, -Fe and two borides (Fe₂B and R_1.1Fe₄B₄) were revealed. The initial phase in all the alloys is recovered after heating in vacuum to a temperature of 990 °C. Full hydrogen desorption occurs in two temperature ranges with the peaks at 200–320 and 630–715 °C.     

Crystallization processes and phase evolution in amorphous Fe–Pt–Nb–B alloys

Fe–Pt system is nowadays widely studied due to its potential applications as magnetic recording media. The hard magnetic FePt L1₀ phase has extremely promising potential as permanent magnet with high magnetocrystalline anisotropy. Of recent interest is also the developing of the hard magnetic phase from an amorphous precursor by appropriate crystallization processes. The melt-spun amorphous Fe₆₈Pt₁₃Nb₂B₁₇ alloy has been submitted to dynamical annealing and its phase transformation during the process has been monitored by differential scanning calorimetry and in situ energy-dispersive X-ray diffraction of the synchrotron radiation. In the first stage of crystallization, -Fe and cubic FePt phases are formed from the amorphous precursor. At around 600 °C superlattice Bragg reflections corresponding to tetragonal FePt are indexed in the XRD spectra and -Fe phase diminishes drastically. Finally, between 900 °C and 975 °C the tetragonal superlattice peaks disappear and cubic FePt phase is formed again. This reversible order–disorder transformation is accompanied by a strong uniaxial lattice expansion of the cubic FePt unit cell. The system show promising features for the co-existence of hard and soft exchange coupled magnetic phases crystallized from FePt-based amorphous precursors.     

The phase diagram of the Yb–Ge system

The phase diagram of the Yb–Ge system was investigated over the whole compositional range by means of differential thermal analysis (DTA), X-ray diffraction (XRD), optical microscopy (LOM) and electron probe microanalysis (EMPA). Besides the already known intermediate phases Yb₂Ge (PbCl₂-type), Yb₅Ge₃ (Mn₅Si₃-type), Yb₁₁Ge₁₀ (Ho₁₁Ge₁₀-type) and Yb₃Ge₅ (Th₃Pd₅-type), two new compounds have been found: Yb₅Ge₄ (Sm₅Ge₄-type) and Yb₃Ge₈, which crystallize with a new triclinic structure type. All the compounds formed in the system have been completely structurally characterized by single crystal determinations.     

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.     

Structure and phase transformations in Fe–Ni–Mn alloys nanostructured by mechanical alloying

Ternary Fe₈₆Ni_xMn_14−x alloys, where x = 0, 2, 4, 6, 8, 10, 12, 14, 16 at.%, were prepared by the mechanical alloying (MA) of elemental powders in a high-energy planetary ball mill. X-ray diffraction analysis and Mössbauer spectroscopy were used to investigate the structure and phase composition of samples. Thermo-magnetic measurements were used to study the phase transformation temperatures. The MA results in the formation of bcc α-Fe and fcc γ-Fe based solid solutions, the hcp phase was not observed after MA. As-milled alloys were annealed with further cooling to ambient or liquid nitrogen temperatures. A significant decrease in martensitic points for the MA alloys was observed that was attributed to the nanocrystalline structure formation.     

Combined thermal desorption spectroscopy,differential scanning calorimetry,scanning electron microscopy and X-ray diffraction study of hydrogen trapping in cold deformed TRIP steel

Thermal desorption spectroscopy (TDS) is a very important tool when evaluating hydrogen–material interactions. It allows a distinction to be drawn between different hydrogen traps in the material based on determination of the peak temperatures for hydrogen desorption during heating. These temperatures depend on the metallurgical and microstructural characteristics of the material and provide important information on the possible mechanisms of hydrogen embrittlement. In the present work TDS experiments were performed on a transformation-induced plasticity (TRIP) steel and combined with an in-depth characterization of the microstructure by scanning electron microscopy, X-ray diffraction and differential scanning calorimetry. The TRIP steel was subjected to different degrees of cold deformation in order to correlate the changing microstructure with the TDS peaks. In order to improve our understanding the results obtained for the TRIP grade steel were also compared with those obtained for electrolytically pure iron, which contained only a limited amount of possible trap sites. Here as well, an increasing number of defects were introduced by cold deformation. Significant differences between the two materials and a significant impact of the degree of cold deformation were observed for TRIP steels, allowing a correlation between the TDS peaks and specific microstructural features.     

Development of nano-structure Cu-Zr alloys by the mechanical alloying process

Cu-Zr alloys have many applications in electrical and welding industries for their high strength and high electrical and thermal conductivities. These alloys are among age-hardenable alloys with capability of having nano-structure with high solute contents obtainable by the mechanical alloying process. In the present work, Cu-Zr alloys have been developed by the mechanical alloying process. Pure copper powders with different amounts of 1, 3 and 6 wt% of commercial pure zirconium powders were mixed. The powder mixtures were milled in a planetary ball mill for different milling times of 4, 12, 48 and 96 h. Ball mill velocity was 250 rpm and ball to powder weight ratio was 10:1. Ethanol was used as process control agent (PCA). The milling atmosphere was protected by argon gas to prevent the oxidation of powders. The milled powders were analysed by XRD technique and were also investigated by SEM observations. Lattice parameters, crystal sizes and internal strains were calculated using XRD data and Williamson-Hall equation. Results showed that the lattice parameter of copper increased with increasing milling time. The microstructure of milled powder particles became finer at longer milling time towards nano-scale structure. SEM observations showed that powder particles took plate-like shapes. Their average size increased initially and reached a maximum value then it decreased at longer milling times. Different zirconium contents had interesting effects on the behavior of powder mixtures during milling.     

Characterization of crystallization kinetics of a Ni- (Cr, Fe, Si, B, C, P) based amorphous brazing alloy by non-isothermal differential scanning calorimetry

The thermal stability and crystallization kinetics of a Ni- (Cr, Si, Fe, B, C, P) based amorphous brazing foil have been investigated by non-isothermal differential scanning calorimetry. The glass transition temperature T_g, is found to be 720 ± 2 K. The amorphous alloy showed three distinct, yet considerably overlapping crystallization transformations with peak crystallization temperatures centered around 739, 778 and 853 ± 2 K, respectively. The solidus and liquidus temperatures are estimated to be 1250 and 1300 ± 2 K, respectively. The apparent activation energies for the three crystallization reactions have been determined using model free isoconversional methods. The typical values for the three crystallization reactions are: 334, 433 and 468 kJ mol⁻¹, respectively. The X-ray diffraction of the crystallized foil revealed the presence of following compounds Ni₃B (Ni₄B₃), CrB, B₂Fe₁₅Si₃, CrSi₂, and Ni_4.5Si₂B.     

Thermal stability and primary phase of Al–Ni(Cu)–La amorphous alloys

Thermal stability and primary phase of Al_85+xNi_9−xLa₆ (x = 0–6) and Al₈₅Ni_9−xCu_xLa₆ (x = 0–9) amorphous alloys were investigated by X-ray diffraction and differential scanning calorimeter. It is revealed that replacing Ni in the Al₈₅Ni₉La₆ alloy by Cu decreases the thermal stability and makes the primary phase change from intermetallic compounds to single fcc-Al as the Cu content reaches and exceeds 4 at.%. When the Ni and La contents are fixed, replacing Al by Cu increases the thermal stability but also promotes the precipitation of single fcc-Al as the primary phase.     

Formation and thermal stability of new Zr–Cu-based bulk glassy alloys with unusual glass-forming ability

The simultaneous addition of Al and Ag to Zr–Cu binary alloys increased in the stabilization of supercooled liquid, the reduced glass transition temperature and γ value, leading to greatly enhance the glass-forming ability (GFA). The Zr–Cu–Ag–Al glassy alloy samples with diameters above 15 mm were obtained in the wide composition range of 42–50 at% Zr, 32–42 at% Cu, 5–10 at% Ag, and 5–12 at% Al. The best GFA was obtained for Zr₄₈Cu₃₆Ag₈Al₈ alloy, and the glassy samples with diameters up to 25 mm were fabricated by an injection copper mold casting. The Zr₄₈Cu₃₆Ag₈Al₈ glassy alloy exhibited high tensile and compressive fracture strength of over 1800 MPa.