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1995, Journal of Magnetism and Magnetic Materials
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Nanocrystallization from Vitrovac amorphous ribbons was studied using Mössbauer spectroscopy, transmission electron microscopy, and differential scanning calorimetry. Co-rich amorphous alloys demonstrated an increase in the residual amorphous phase's Fe content following crystallization. This resulted in enhanced hyperfine fields and Curie temperature, while crystallization of grains smaller than 15 nm led to significant softening of magnetic properties. Controlled thermal annealing at temperatures lower than crystallization temperature increased initial magnetic permeability by five times. The findings contribute to understanding magnetic behavior in these materials.
Intermetallics, 2000
The mechanism of nanocrystallisation of the amorphous Fe 72 Cu 1 Nb 4.5 Si 13.5 B 9 alloy has been studied with particular attention to the early stages of crystallisation. The specimens have been nanocrystallised by furnace (FA) and current (CA) annealing and analysed by MoÈ ssbauer spectroscopy. X-ray scattering, using the beamline 5.2L at Elettra Synchrotron Source, Trieste, has been carried out on the same FA and CA samples, as well as on a previously untreated sample current heated in situ. It is found that for the same amount of nanocrystalline phase, the crystallite size in CA samples does not dier signi®cantly from that in FA samples. Analysis of the MoÈ ssbauer spectra shows that in FA and CA samples the nanocrystalline grains consist of non-stoichiometric partially disordered Fe 3 Si phase, and that there is an indication of the presence of boron atoms in the nanocrystals of CA samples. This implies a lower segregation of boron atoms or of borides at the boundaries of nanocrystallites of CA samples and can be connected to their lower brittleness. #
Journal of Non-Crystalline Solids, 2003
The time-temperature dependence of Curie temperature (T C ) was determined by the DSC method for amorphous Fe 73:5 Cu 1 Nb 3 Si 15:5 B 7 ribbon-shaped alloy on annealing below the crystallization temperature. Relaxation of atomic structure of the amorphous phase on annealing was accompanied by an increase of T C . The r-shaped time dependence was not characterized, however, by a single value of T C , since long-time annealing of amorphous samples resulted in a slow increase of T C at each temperature. The appearance of two heat capacity maxima observed after short-time annealing at the pre-crystallization temperature was associated with two Curie points (T C1 and T C2 ). These peaks were related to clustering inside the amorphous phase and to separation into two phases with different chemical compositions. Further annealing resulted in a-Fe nuclei appearance in the amorphous phase and consequently in the disappearance of iron-rich clusters.
Journal of Alloys and Compounds, 2004
High-temperature in situ 57 Fe Mössbauer spectroscopy was used to investigate the nanocrystallization process in Fe 73.5 Si 13.5 B 9 Cu 1 Nb 1 X 2 (X = Zr, Nb, Mo and V) amorphous alloys. The Mössbauer spectra were taken at temperatures where only the amorphous phase is found in a paramagnetic state, allowing an accurate resolution between the amorphous and crystalline phases presented in the annealed ribbons. The Johnson-Mehl-Avrami theory was used to describe the increase of the crystalline fraction (in vol.%) as a function of the annealing time. The volume fraction of the iron-silicate nanocrystalline phase, found in each of the alloys annealed under similar conditions, increases in the sequence Zr < Nb < Mo < V. The value of the Avrami exponent, determined for each alloy, is near 1, indicating a controlled diffusion process with a nucleation rate close to zero. An activation energy of 3 eV was found for the studied alloys. .pe (V.A. Peña Rodríguez).
Journal of Alloys and …, 2011
Dependence of Curie temperature (Tc) on time and temperature of annealing for Finemet-type amorphous alloys is studied by DSC. Structural relaxation of an amorphous phase at annealing is accompanied by increase of Tc. The-shaped time dependencies, however, are not characterized by the definite final value of Tc: long-term annealing of amorphous phase results in continuation of slow increase of Tc for every temperature. Apparent values of activation energy of relaxation were evaluated from the Tc time-temperature dependencies. It is found that the average value of activation energy increases with progress of the relaxation process. Correlation of the Tc data with structural alterations reflects redistribution of components in amorphous phase during annealing. Further increase of the annealing temperature results in precipitation of ␣-Fe(Si) nanograins in an amorphous matrix, that accompanied by gradual degradation of corresponding to Tc heat capacity peak. DSC measurements of Tc allow to detect the starting moment of amorphous phase crystallization.
Materials Science and Engineering: A, 1991
The structure of ferromagnetic amorphous alloys Fe73.sX1Nb3Si13.sBg, with X = Cu, Au, Pt, Pd, has been investigated by TEM, resistometry, dilatometry and magnetic measurements. Nanocrystalline grain formation is observed in these alloys upon crystallization. Ultrafine grains are preserved in alloys with additives which are insoluble in b.c.c.-Fe (Cu, Au), thus forming, together with niobium, a relatively stable interfacial barrier around the grains preventing their growth. In alloys with additives soluble in b.c.e.-Fe, grain sizes increase upon prolonged annealing.
IEEE Transactions on Magnetics, 1983
Changes in the Curie temperture, Tc, due to various heat treatments were studied for an amorphous alloy Fe32Ni36Cr14P12Bg. It was found that Tc approaches equilibrium values after prolonged annealing, and 'the kinetics can be described by the distributed activation energies. The activation energy spectrum, however, depends upon the prior quenching condition in a manner similar to that observed for the reorientation of the induced anisotropy and internal friction.
Journal of Metastable and Nanocrystalline Materials, 2004
In the present work the Fe 63 Nb 10 Al 4 Si 3 B 20 (%at) alloy has been processed by melt spinning process with the aim of obtain amorphous ribbon and study the crystallization sequence through annealing in suitable temperatures. A lot of effort has been done in the search for new compositions which provide very fine nanocrystalline structures in ferromagnetic amorphous alloys in order to improve soft magnetic properties. This alloy was obtained with low cost Fe-Nb and Fe-(Al,Si)-B master alloys to evaluate the influence of impurity elements. Ribbons were produced at a tangential wheel speed of 56 m/s. The amorphous ribbon was further analyzed by differential scanning calorimetry (DSC), X-ray diffractometry (XRD) and transmission electron microscopy (TEM), for the characterization of crystalline phases formed in each crystallization peak of DSC analysis. The thermogram of DSC analysis showed four exothermic peaks with the onset crystallization T x = 560ºC. The combination of X-ray diffractograms and selected area diffraction pattern (SAPD) on TEM was used to identify the crystallized phases. Annealed samples showed the following phases: (first peak) α-Fe nanocrystals embebed in an amorphous matrix; (second peak) α-Fe nanocrystals + Fe 23 B 6 intermetallic embebed in an amorphous matrix; (third peak) α-Fe nanocrystals + FeNbB intermetallic embebed in an amorphous matrix; (fourth peak) α-Fe + FeNbB + FeB phases.
International Journal of Materials Research, 2015
Test samples of the alloy Fe61Co10Y8W1B20 were fabricated in the form of both amorphous ribbons and bulk amor-phous plates. The structure, microstructure and magnetic properties of samples in the as-quenched state and after annealing were investigated. The aim of the paper is to show the effect of the thermal treatment on the structural changes occurring in the amorphous state. The thermal treatment, performed at well below the crystallisation temperature, did not cause crystallisation. In the investigated amorphous alloys it has been found that, after a specific thermal treatment, structural relaxation occurs in the presence of structural defects, such as quasidislocational dipoles. Also, supporting the microscopy investigations with measurements of the magnetic properties can be extremely beneficial for facilitating description of the real structure and properties of the amorphous alloys; further, this testing combination offers the possibility for designing the optimal applicatio...
Intermetallics, 2012
Materiali in tehnologije, 2017
This paper presents the results of research into a bulk amorphous alloy based on Fe. Samples with the composition Fe61Co10Y8Mo1B20 were prepared in the form of plates using an injection-casting method. The samples were then subjected to an isothermal annealing process (at less than the crystallization temperature) of 700 K for 1 h and 770 K for 3.5 h The structures of the samples were investigated, both in the state after solidification and following the heat treatment, using X-ray diffraction (XRD) and Mössbauer spectroscopy. The results confirmed that the samples, both after solidification and after annealing, were amorphous. Magnetic measurements were carried out using a vibrating-sample magnetometer (VSM) with magnetic fields of up to 2 T. Based on these measurements, the effect of the isothermal annealing process on the magnetic properties was defined, including the saturation magnetization μ0Ms and coercive field Hc. Using the Kronmüller theory, the initial magnetization curves were analysed in the area of approach to ferromagnetic saturation. On the basis of this theory, the quantity and quality of the structural defects were defined; these defects play a critical role in the magnetization process in high magnetic fields. Following this study, the sample annealed at 770 K for 1 h was found to feature a relatively low coercive field and the higher value of magnetization saturation. Linear defects, the so-called quasidislocational dipoles, played the leading role in the process of magnetization of the test samples. Keywords: bulk amorphous alloys, structure, soft magnetic properties, defectŝ lanek predstavlja rezultate raziskave masivne amorfne zlitine na osnovi Fe. Vzorci s sestavo Fe61Co10Y8Mo1B20 so bili pripravljeni v obliki plo{~, s pomo~jo tla~nega litja. Vzorci so bili izotermno`arjeni 1 h (pri temperaturi ni`ji od temperature kristalizacije) na 700 K in 3,5 h na 770 K. Preiskana je bila struktura vzorcev, v stanju po strjevanju in po toplotni obdelavi. Uporabljena je bila rentgenska difrakcija (XRD) in Mössbauerjeva spektroskopija. Rezultati so potrdili, da so bili vzorci po strjevanju in po`arjenju v amorfnem stanju. Magnetne meritve so bile izvedene s pomo~jo magnetometra z vibriranjem vzorca (VSM) v magnetnih poljih jakosti do 2 T. Na osnovi meritev je bil dolo~en vpliv izotermnega`arjenja na magnetne lastnosti, vklju~no z nasi~eno magnetizacijo μ0Ms in koercitivnim poljem Hc. Z uporabo Kronmüllerjeve teorije so bile analizirane za~etne krivulje magnetizacije blizu podro~ja feromagnetnega nasi~enja. Na osnovi te teorije je bila dolo~ena koli~ina in kakovost strukturnih napak; te napake igrajo klju~no vlogo pri procesu magnetizacije v mo~nih magnetnih poljih. Na podlagi te {tudije je bilo ugotovljeno, da vzorci`arjeni 1 h ka`ejo relativno {ibko koercitivno polje in visoko vrednost nasi~ene magnetizacije. Linearne napake, imenovane kvazi-dislokacijski dipoli, igrajo vodilno vlogo pri procesu magnetizacije preizku{anih vzorcev. Klju~ne besede: masivne amorfne zlitine, struktura, mehko magnetne lastnosti, napake
Hyperfine Interactions, 1992
Journal of Applied Physics, 2000
Specimens of the amorphous Fe 72 Cu 1 Nb 4.5 Si 13.5 B 9 alloy have been nanocrystallized by furnace ͑FA͒ and current ͑CA͒ annealing and analyzed by simultaneous small-angle ͑SAXS͒ and wide-angle ͑WAXS͒ x-ray scattering using the beam-line 5.2L at Elettra Synchrotron Source, Trieste. The analysis has been carried out also dynamically on untreated samples current heated in situ. Significant differences in the SAXS regime have been observed between the FA and CA samples having the same amount of nanocrystallization as determined from previous WAXS and Mössbauer measurements. These differences can be attributed to a lower contrast of the nanocrystallites in the CA samples as compared to FA samples. The Mössbauer spectra show that in FA and CA samples the nanocrystalline grains consist of a nonstoichiometric partially disordered Fe 3 Si phase, and indicate the presence of boron atoms in the nanocrystals of CA samples. This is in agreement with the lower contrast found by SAXS and implies a lower segregation of boron atoms and/or of borides at the boundaries of nanocrystallites of CA samples, accounting for their lower brittleness.
World Journal of Nano Science and Engineering, 2015
Iron-based amorphous alloys have attracted technological and scientific interests due to their excellent soft magnetic properties. The typical nanocrystalline alloy with the composition of Fe 73.5 Cu 1 Nb 3 Si 13.5 B 9 known as FINEMENT has been studied for structural properties analysis. Recently, it is found that after proper annealing the amorphous alloy like Fe 73.5 Cu 1 Nb 3 Si 13.5 B 9 has a transition to the nanocrystalline state, thus exhibiting good magnetic properties. The alloy in the form of ribbon of 10 mm width and 25mm thickness with the composition of Fe 73.5 Cu 1 Nb 3 Si 13.5 B 9 was prepared by rapid quenching method. The prepared ribbon sample has been annealed for 30 min in a controlled way in the temperature range 490˚C-680˚C. By analyzing X-ray diffraction (XRD) patterns, various structural parameters such as lattice parameters, grain size and silicon content of the nanocrystalline Fe(Si) grains, crystallization behavior and nanocrystalline phase formation have been investigated. In the nanocrystalline state, Cu helps the nucleation of α-Fe(Si) grains while Nb controls their growth, Si and B has been used as glass forming materials. Thus on the residual amorphous, the nanometric Fe(Si) grains develops. From broadening of fundamental peaks, the optimum grain size has been determined in the range of 7-23 nm.
Journal of Alloys and Compounds, 2014
In this paper, the influence of production method on the basic magnetic properties and structure of amorphous alloys, in the forms of ribbons and plates, was investigated. The samples used in the investigations were obtained by three different production methods: ultrafast cooling of the liquid alloy on a rotating copper wheel (the melt-spinning method), and the injection or suction of the molten alloy into a water-cooled copper die injection-and suction-casting, respectively. The structure of the resulting samples of Fe 61 Co 10 Y 8 Nb 1 B 20 alloy was investigated by means of X-ray diffractometry, Mössbauer spectroscopy and scanning electron microscopy. The results of the microstructural investigations confirmed that the obtained samples were amorphous and without crystalline precipitations. The images from the scanning electron microscope were typical for amorphous materials. Magnetic measurements were performed using a vibrating sample magnetometer (VSM) using magnetic fields of up to 2 T. The highest value of the saturation magnetization was achieved for the sample which was in the form of a ribbon. The values of this parameter for the samples which were in the form of plates were similar to each other, regardless of the production method. The values of the coercivity showed much greater differences, depending on the production method. The smallest value of coercivity was found for the sample in plate-form obtained by injection-casting; this is connected with the highest value of structural relaxation in the investigated material.
2013
The nanocrystallization of Co67Fe4Cr7Si8B14 amorphous ribbons which prepared by planar flow melt spinning process (PFMS) was investigated. Crystallization of the ribbons was studied by differential thermal analysis (DTA), X-ray diffraction (XRD) and transmission electron microscopy (TEM). The DTA result of amorphous ribbon at heating rate of 10 ̊C/min showed occurrence of phase transitions in two stages. The ribbons were isothermally annealed for 30 minutes in argon atmosphere at different temperatures between 300 and 650oC with 25oC steps. The magnetic properties of annealed samples were measured using a vibrating sample magnetometer (VSM). The VSM results revealed that optimum soft magnetic properties occurred at 400oC. XRD patterns showed that the samples isothermally annealed up to 450oC were amorphous, while TEM results at 400oC indicated 7-8 nm mean size nanocrytallites in amorphous matrix and size of the nanocrystallites increased by increasing temperature. Also by X-ray diff...
2005
Magnetic behavior, microstructural evolution, and amorphization studies of Fe 42 Ni 28 Zr 8 Ta 2 B 10 C 10 alloy, synthetized by mechanical alloying, were investigated. The non-equilibrium microstructure originated from a grain size reduction to about 2.5 nm indicated by X-ray diffraction and the introduction of internal strain up to 3.8%. The results showed that as the milling time increased the amorphous phase became dominant and reached about 92 wt.% at 176 h. The magnetic measurements which were obtained by vibrating sample magnetometer, showed an increase in saturation magnetization up to 12 h and then a decrease until 66 h followed by a slow increase. Simultaneously, the coercivity increased, decreased and finally reached a constant level of about 24 Oe. The value of coercivity obtained in the present study is less than the values reported for the widely investigated mechanically alloyed Fe-Ni-Zr-B alloys, which shows this alloy is a very good soft magnet.
Journal of Bangladesh Academy of Sciences, 2016
To observe the impact of the annealing time on the alloy structure and ultra-soft magnetic properties of Fe 75.5 Si 13.5 Cu 1 Nb 1 B 9 , the alloy was annealed in a controlled way in the temperature range 475-600°C for different annealing time from 5 to 30 min. Amorphosity of the ribbon and nanocrystalline state was evaluated by X-ray diffraction. Grain size and Si content increase with increasing annealing temperature and time; on the other hand lattice parameter decrease with increasing annealing temperature and time. The maximum permeability was observed at annealing temperature Ta = 525°C for 15 min, and thereafter it starts to decreases. Saturation magnetization increases with annealing temperature Ta for the samples and finally decreases during annealing at a temperature much higher than peak crystallization temperature. The results of the experimental observations are explained on the basis of existing theories of nanocrystalline amorphous metallic ribbons.
Journal of Magnetism and Magnetic Materials, 2001
We report here a large (300}400 K) increase of the decoupling temperature (¹?K ) with increasing crystalline fraction in Nanoperm-type alloys. This is in contrast to the Finemet-type alloys where ¹?K varies some tens of K only around the original as-cast amorphous ¹ when the amorphous precursor is annealed around the "rst crystallization peak. H and M /M , versus ¹ measurements have been used to monitor the exchange decoupling of the nanosized particles, because these parameters are more sensitive to decoupling than M and , which show no characteristic change at the decoupling. This enhancement of ¹?K has been tentatively attributed to the increasing boron content of the residual amorphous matrix whereas the zirconium atoms agglomerate in the grain boundary region.
Journal of Alloys and Compounds, 2011
PACS: 75.50.Bb 75.50.Kj 65.60+a 75.60 Ej 76.80.+y 61.05.C 61.05.Qr Keywords: Fe and its alloys Amorphous magnetic materials Thermal properties of amorphous solids and glasses Magnetization curves Hysteresis Mössbauer effect X-ray diffraction Mössbauer spectroscopy
physica status solidi (a), 2002
The influence of the relative weight of Ge and Al and different annealing temperatures on the evolution of the internal structure of Fe-Si-B-Ge-Nb-Cu-Al ribbons is studied. The iron environment in the amorphous and crystallized alloys is investigated employing Mö ssbauer spectroscopy and the evolution of the crystallization process is followed by X-ray diffraction. The ribbons have been obtained by means of the melt spinning technique. The effect of the change in mechanical and magnetic properties is analyzed and the results are compared with previous works on Fe 73.5 Si 22.5--x B x Nb 3 Cu 1 and (6 x 12) ribbons.
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