Nanocrystallization-induced structural evolution of intergranular amorphous phase in Fe78B13Si9 alloy

The nanocrystallization-induced structural evolution of the intergranular amorphous phase in a Fe₇₈B₁₃Si₉ alloy was investigated by X-ray diffraction (XRD) measurements, transmission electron microscopy (TEM), and positron annihilation spectroscopy. Crystallization occurs at 773 K, where nanocrystallites of α-Fe with an average grain size of a few tens of nanometers are formed in an amorphous matrix. With increasing annealing temperature up to 973 K, the average grain size increases up to ∼80 nm. In the as-prepared sample corresponding to an amorphous precursor, more than 90% of the positrons are localized at vacancy-sized free volumes dominantly surrounded by Fe atoms and other positrons are trapped by microvoids. Along with the appearance of nanocrystallites and their growth due to annealing, the concentration of microvoids is increased in the intergranular amorphous phase.     

Plastic deformation behavior of amorphous Fe78Si9B13 alloy at elevated temperature

The plastic deformation behavior of amorphous Fe₇₈Si₉B₁₃ alloy was investigated under uniaxial tension and gas pressure bulging. The deformed specimens were studied by means of XRD and SEM. It is shown that amorphous Fe₇₈Si₉B₁₃ ribbon has good deformation ability in the temperature range from 450 °C to 500 °C. The elongation of 36.3% and the relative bulging height (RBH) of 0.45 were obtained at 500 °C. In the uniaxial tension test, the amount of the crystalline α-Fe phase increases with deformation temperature below the crystallization temperature, which also suggests that the tensile stress promotes the crystallization of amorphous Fe₇₈Si₉B₁₃ ribbon. The suitable gas pressure bulging conditions for the specimens are 500 °C, 3.4 MPa and 30 min.     

In-situ crystallization of amorphous Fe73−xNbxAl4Si3B20 alloys through synchrotron radiation

In the present work Fe_73−xNb_xAl₄Si₃B₂₀ (x = 5, 10) alloys have been processed by melt-spinning with the aim of studying the crystallization sequence through annealing in suitable temperatures. Melt-spun ribbons were characterized by differential scanning calorimetry (DSC), X-ray diffractometry (XRD) through Cu-Kα (λ = 1.54 Å) and synchrotron radiation (λ = 1.77 Å) and transmission electron microscopy (TEM). Soft magnetic properties were measured through the hysteresis loop tracer. In-situ XRD through synchrotron radiation was very accurate in phase identification. Fe_73−xNb_xAl₄Si₃B₂₀ (x = 5, 10) alloys showed the possibility of forming ferromagnetic amorphous alloys composed of commercial Fe-based master alloys with fine nanocrystalline structure and good soft magnetic properties.     

Glass-to-crystalline transformation in rapidly quenched Fe78B9Si13 ferromagnetic alloy

Calorimetric studies of the ferromagnetic Curie temperature T_c, and the crystallization kinetics of the metallic glass Fe₇₈B₉Si₁₃ have been performed in an attempt to elucidate the possibility of reversible relaxation processes near T_c and the crystallization mechanisms taking place. From the change of T_c with heating rate and on annealing it appears that ageing irreversibly increases the Curie temperature. Crystallization is thermally activated following an Arrhenius behaviour and proceeds in two stages, the best fit to the experimental data for each stage of crystallization has been obtained by use of a Johnson-Mehl-Avrami-Erofe'ev equation. The effective activation energy and the kinetic exponent are respectively E = (4.7 ± 0.1) eV, n = 2.0 ± 0.2 for the first and E = (4.5 ± 0.1) eV, n = 4.0 ± 0.2 for the second stage of crystallization. From these results it appears that the mechanisms of crystallization are quite different in both stages.     

Nanocrystallization and structure of Fe78.5Ni1.0Mo0.5Si6.0B14.0 amorphous alloy

The effect of Ni and Mo alloying additions on crystallization of an Fe–Si–B based amorphous alloy was studied by applying various experimental techniques – DSC, XRD and TEM. It was shown that both alloying additions Ni and Mo change the crystallization temperature as well as the activation energy of primary crystallization. The phases formed during primary crystallization for the Fe₈₀Si₆B₁₄ and Fe_78.5Ni₁Mo_0.5Si₆B₁₄ alloys were the same, however the morphologies were significantly different. The addition of 1.0 at.% of Ni and 0.5 at.% Mo changed the crystallization mechanism and the type of formed phases. Such additions also resulted in formation of nanocrystals. The kinetic and thermodynamic characteristics of annealed specimens of amorphous metallic Fe₈₀Si₆B₁₄ and Fe_78.5Ni₁Mo_0.5Si₆B₁₄ alloys were established. These characteristics were determined based on measurements of instantaneous changes of electrical strength. It was shown that the method of electromotive force measurements was more sensitive to structural changes and the phase composition of amorphous metallic electrodes in comparison with the X-ray method.     

Magnetic behaviors of amorphous Fe78Si9B13 thin films prepared by pulsed laser deposition

Amorphous magnetic thin films have been deposited onto BK-7 substrates using the pulsed laser deposition technique. The source material irradiated by the laser was a pack of amorphous ribbons of composition Fe₇₈Si₉B₁₃. The structural properties of thin films were investigated and a large number of droplets were observed in the magnetic layers. Electric current passing through the films causes significant deformation of droplets and consequently changes the magnetic thin films characteristics. Magnetic properties evolution after electrical processing was investigated using magneto-optical Kerr effect.     

Stability and crystallization of Fe-Co-Nb-B amorphous alloys

New soft magnetic amorphous alloys with a wide supercooled liquid region were obtained by increasing the boron content (up to 30 at.%) and by addition of cobalt (composition range between 5 and 42 at.%) in FeNbB based materials. Upon thermal treatments, the stability and the crystallization behavior of Fe₅₂Co₁₀Nb₈B₃₀ and Fe₂₂Co₄₀Nb₈B₃₀ have been studied by using X-ray diffraction (XRD) and transmission electron microscopy (TEM). On the other hand, the Curie temperature change, T_c, of the remaining amorphous phases has been determined by thermomagnetic analysis (TMG). Sub-micrometric fcc-(Co,Fe) and fcc-(Fe,Co)₂₁Nb₂B₆ grains were observed to crystallize at a relatively high temperature (950-970 K) providing an excellent stability of the amorphous states. Due to the partitioning behavior, occurring during crystallization, the Curie temperature of the remaining amorphous structure is observed to increase in the case of the Fe₅₂Co₁₀Nb₈B₃₀ composition while a decrease of T_c to the lower temperatures is observed with the Fe₂₂Co₄₀Nb₈B₃₀ composition.     

The use of flow behavior and thermal expansion to monitor structural change of amorphous Fe78Si9B13 ribbon

Samples of the amorphous Fe₇₈Si₉B₁₃ ribbon were annealed isothermally and isochronally under different tensile stresses. These samples were also investigated using thermal expansion tests, DSC and XRD methods. The results show that a structural transition similar to the glass transition was found using thermal expansion method. Comparing the XRD patterns of the tensile stress annealed samples with those of stress free annealed samples, it is suggested that tensile stress promotes the crystallization.     

Complex primary crystallization kinetics of amorphous Finemet alloy

The complex primary crystallization kinetics of the amorphous Finemet soft magnetic alloys has been analyzed by non-isothermal DSC measurements. The local activation energies E_c(α) were determined by an isoconversional method without assuming the kinetic model function and its average value was about 383 kJ/mol. The nucleation activation energy E_n and growth activation energy E_g were 425 and 333 kJ/mol, respectively. And the apparent local activation energies E_c can be expressed by E_n and E_g as follows: E_c = aE_n + bE_g. The local Avrami exponents lies between 1 and 2 in a wide range of 0.2 < α < 0.9, and it indicates that dominating crystallization mechanism in the non-isothermal primary crystallization of amorphous Finemet alloy is one dimensional growth at a near-zero nucleation rate for surface crystallization. The significant variation of local Avrami exponent and local activation energy for primary crystallization with crystallized volume fraction demonstrates that the primary crystallization kinetics of amorphous Finemet alloy varies at different stages. In addition, the variable local activation energies E_c(α) and local Avrami exponents n(α) are applicable and correct in describing the primary crystallization process of the amorphous Finemet alloy according to the theoretical DSC curve simulation.     

Structural and dynamical properties of Fe78Si9B13 alloy during rapid quenching by first principles molecular dynamic simulation

Structural evolution of the Fe₇₈Si₉B₁₃ alloy during rapid quenching was investigated by ab initio molecular dynamics simulation. The second peak splitting has been perceived even at 1473 K in the partial pair correlation functions though not in the total pair correlation function. The (0, 3, 6, 0) polyhedra are abundant in the liquid state while the distorted (0, 3, 6, 0) polyhedra are the featured local structure around B atoms in the amorphous state. The diffusion coefficients of the three elements are evaluated to understand the dynamics of quenching. From 1173 to 873 K the three coefficients are coherent. We think this temperature range corresponds to the supercooled liquid region, and 873 K serves as the glass transition temperature.     

Magnetostatic properties of amorphous and nanostructured Fe73.5Si13.5B9Cu1Nb3 wires

We present the results of experimental investigations of magnetostatic properties of Fe-based amorphous wires with diameter about 100 μm. The samples were annealed at different conditions. The as-quenched sample had a weak increase (about 5%) of the magnetization with magnetic field decrease – the negative differential magnetic permeability could be observed in its hysteresis loops. The coercive force was about 0.2 Oe. The conventional annealing decreased the value of the saturation field down to 5 Oe without change of the coercive force value. When the annealing was accompanied with torsion stress the coercive force became less than 50 mOe. After the current annealing any peculiarities disappeared in magnetization in a weak magnetic field.     

The formation and crystallization of amorphous Al65Fe20Zr15

Amorphous Al₆₅Fe₂₀Zr₁₅ alloy has been prepared by mechanical alloying. The as-milled powders were analyzed by XRD and DTA. The fully amorphous alloy was identified by the hallo rings of XRD pattern. The effective activation energy of crystallization was estimated with modified Kissinger’s plot and it is 321.0 kJ/mol evaluated from the peak temperature of crystallization. The product phases of crystallization composed of Al₃Zr, Al₈₂Fe₁₈, AlFeZr and an unidentified phase. The crystallization kinetics was also discussed by using the isochronal DTA scans and the values of corresponding kinetic parameters were determined.     

Impact of amorphous Ge thin layer at the amorphous Si/Al interface on Al-induced crystallization

We investigated the impact of an amorphous Ge (a-Ge) thin layer inserted at the amorphous Si (a-Si)/Al interface on Al-induced crystallization. In situ observation of the growth process clarified that the nucleation rate is drastically reduced by insertion of a-Ge, which led to increase in the average size of crystal grains. This was interpreted as resulting from decrease in the driving force of crystallization, mainly due to the larger solubility of Ge in Al than that of Si in Al. The obtained films were SiGe alloys with lateral distribution of Ge content, and its origin is discussed based on the two-step nucleation process.     

Atomic diffusion of boron and other constituents in amorphous Si–B–C–N

The self-diffusion of boron is studied between 1550 and 1700 °C in polymer-derived amorphous solids of composition Si₃BC_4.3N₂. Ion implanted stable ¹⁰B isotopes are used as tracers and secondary ion mass spectrometry for depth profiling. The experimentally determined diffusivities obey an Arrhenius behavior with a high activation enthalpy of ΔH = (7.3 ± 1.3) eV and a high pre-exponential factor of D₀ = 1.6 m²/s. The results are discussed in relation to the diffusivities of the other constituents (Si, C, N) and possible diffusion mechanism are suggested.     

Trap-limited diffusion of hydrogen in precursor derived amorphous Si–B–C–N-ceramics

The tracer diffusion of hydrogen is studied in precursor derived amorphous Si–C–N and Si–B–C–N ceramics using deuterium as a tracer and secondary ion mass spectrometry (SIMS). Since the amorphous ceramics are separated in carbon rich phases (amorphous carbon and amorphous C(BN)_x, respectively) and silicon rich phases (amorphous Si₃N₄ and amorphous Si_3+(1/4)xC_xN_4−x, respectively) we additionally measured the diffusivities of hydrogen in amorphous carbon, in amorphous SiC and in amorphous C–B–N films. The silicon rich phases are identified as diffusion paths for hydrogen in the precursor derived ceramics. Diffusion of hydrogen in these materials is explained with a trap limited diffusion mechanism with a single trap level. We found activation enthalpies of about 2 eV for the precursor derived ceramics, where the activation enthalpy is the sum of a migration enthalpy and a binding enthalpy. The low values for the pre-exponential factors of less than 10⁻⁷ m²/s can be explained with an appropriate expression for the entropy factor.     

Influence of Gd and Fe on crystallization of Al87Y5Ni8 amorphous alloy

Crystallization of amorphous Al-based alloys (Al-Y-Gd-Ni-Fe) was investigated by applying differential scanning calorimetry (DSC), X-ray diffraction (XRD) and high resolution electron microscopy (HREM). It was shown that the crystallization in the examined alloys proceeds in three stages (DSC maxima). The two first stages are attributed to formation of solid solution of fcc Al(RE) nanograins in amorphous matrix. In the third stage the precipitation of ternary compound Al₁₉Ni₅RE₃ of the orthorhombic Al₁₉Ni₅Gd₃-type structure was observed. A partial substitution of Ni by Fe causes a change of stoichiometry and crystal structure of the ternary compounds: Al₈TM₄RE (TM = Fe, Ni; RE = Y, Gd) of the tetragonal ThMn₁₂ (Al₈Mn₄Ce)-type structure. A partial replacing of Y atoms by Gd in the Al₈₇Y₅Ni₈ based alloy shifts the Al(RE) nanocrystallization to lower temperatures. In contrast to this a partial replacing of Ni by Fe shifts the nanocrystallization to higher temperatures.     

Crystallization of metastable phases in the Pd83Si17 amorphous alloy

The crystallization of the Pd₈₃Si₁₇ amorphous alloy started by formation of small crystallites. By comparisons of selected area electron diffraction patterns from the crystallites and patterns calculated from generated models we found that the first observed structures coincide with long range vacancy ordered structures derived from CsCl-type structure, known as τ-structures. The Pd atoms are in the corners and the Si atoms or vacancies are in the centers of basic cubic cell, respectively. It is possible to interpret the formation of these transition structures as consequence of occurrence of small areas with different chemical composition present in original amorphous structure as a result of rapid quenching. After ageing the τ-structures transform by diffusion to the stable Pd₉Si₂ structure.     

Effects of sintering temperature on microstructure and property evolution of Fe81Cu2Nb3Si14 soft magnetic materials fabricated from amorphous melt-spun ribbons by spark plasma sintering technique

Bulk Fe₈₁Cu₂Nb₃Si₁₄ soft magnetic materials were fabricated by spark plasma sintering (SPS) of amorphous powder, which was prepared by ball milling of melt-spun ribbons. Effects of sintering temperature on the evolution of microstructure and related properties were systematically investigated. Results show that the as-milled powders exhibit similar microstructure and thermal property in comparison with the original melt-spun ribbons. With an increase in the sintering temperature, the relative density, microhardness and saturation magnetization of the sintered samples improved obviously, but the coercive force decreased at the beginning and then increased with the increase of sintering temperature. The sintered samples exhibit typical soft magnetic characteristic. The desirable soft magnetic property of the sintered samples was achieved by SPS at 630 °C. Meanwhile, microstructure and densification behaviors of the sintered samples were also investigated.     

Effect of Al substitution on the magnetic properties of amorphous Fe73.5Cu1Mo3Si13.5−xAlxB9 alloy

We have synthesized FINEMET type amorphous Fe_73.5Cu₁Mo₃Si_13.5−xAl_xB₉ alloy by the single wheel melt spinning technique. The effect of Al substitution on the magnetic properties has been studied using a vibrating sample magnetometer, SQUID and Mössbauer spectroscopy. Magnetization and Curie temperature of the amorphous phase of the alloys were found to decrease with Al concentration. The results are attributed to the dilution effect of Al on the magnetic moment of Fe and to the increase in Fe–Fe interaction distance resulting in the weakening of exchange interaction.