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Öğe A single step synthesis by mechanical alloying and characterization of nanostructured Fe2B of high magnetic moment(Elsevier Sci Ltd, 2021) Şimşek, Telem; Avar, Barış; Şimşek, Tuncay; Yıldız, Büşra; Chattopadhyay, Arun K.; Özcan, ŞadanThis paper delineates a single-step production method of nanostructured diiron boride (Fe2B) and its structural, magnetic and magnetothermal properties. Structurally Fe2B resembles the tetragonal copper aluminide, CuAl2. The samples of nanostructured Fe2B were synthesized by milling Fe and B powders without any pre-treatment. Single phase Fe2B nanoparticles were successfully produced with the crystallite sizes of 68 and 46 nm after milling the powders for 10 h and 20 h, respectively. The saturation magnetization of the samples was found to decrease with increased milling time indicating that the surface spin disorder plays a crucial role in the magnetic properties. The highest saturation magnetization (Ms) of 141 emu/g with low coercivity (Hc) of 48 Oe was obtained for the 10 h milled sample of Fe2B, whereas the 20 h milled sample exhibited Ms and Hc as 129 emu/g and 149 Oe. This paper also presents a detailed information on the total and atom projected densities of state functions as well as the magnetic moment contribution of the individual atoms of Fe and B in Fe2B explaining the strong room temperature ferromagnetic properties contributed by the large number of unpaired 3 d electrons in Fe. The magnetothermal properties of the as-made Fe2B nanocrystals of high magnetic moment were investigated by measuring the rise in temperature as a function of time in the presence of AC magnetic fields. The magnetic Fe2B nanocrystals show significant thermal response with the high specific absorption rate of 172 W/g, demonstrating the advantages of using Fe2B nanocrystals for the application in magnetic fluid therapy for hyperthermia.Öğe Solid-State Synthesis and Characterization of the Stable Nanostructured Ni21Ti2B6 Phase(Wiley-V C H Verlag Gmbh, 2021) Şimşek, Tuncay; Avar, Barış; Özcan, Şadan; Chattopadhyay, Arun K.; Kalkan, BoraHerein, nanostructured ternary Ni-Ti-B alloy synthesized by mechanical alloying from the elemental Ni, Ti, and B powders by high energy ball milling is described. The synthesized alloy of nominal composition of Ni70Ti10B20 results in the formation of a unique stable phase of Ni21Ti2B6, which happens to be stoichiometrically very close to Ni70Ti10B20 in the cubic symmetry. The synthesized alloy samples also show amorphization together with the formation of nanocrystalline phases of Ni21Ti2B6 at both early and later stages of the alloying process. Thermal analysis carried out on Ni70Ti10B20 induces crystallinity and reveals the formation of crystalline Ni-Ti-B ternary alloy, Ni21Ti2B6, above 523 K, confirming the stability of the ternary crystalline phase of the alloy. The magnetic saturation of the alloy is measured as 0.95 emu g(-1) for the starting amorphous phase that increases to 9.05 emu g(-1) for the crystalline phase upon annealing. Correspondingly, the coercivity value for the annealed sample is reduced to 70 Oe from 194 Oe for the amorphous phase. This is the first time that an evidence of the stable crystalline Ni-Ti-B ternary alloy is reported.Öğe Structural stability of mechanically alloyed amorphous (FeCoNi)70Ti10B20 under high-temperature and high-pressure(Elsevier Science Sa, 2021) Avar, Barış; Şimşek, Tuncay; Özcan, Şadan; Chattopadhyay, Arun K.; Kalkan, BoraNanostructured (FeCoNi)(70)Ti10B20 (at%) alloy was synthesized by mechanical alloying from elemental powder mixture of Fe, Co, Ni, Ti and B using ball milling. The effect of ball milling time on the evolution of structure and morphology was investigated by X-ray diffraction, scanning and transmission electron microscopy and differential thermal analysis. It was observed that the formation of solid solution of (FeCoNi)(70)Ti10B20 started from the very onset of the milling process. Crystallite size and lattice strains seemed to be leveled off after 20 h of milling with no further major changes. The milling process for longer periods introduced severe plastic deformations causing formation of amorphous phase of (FeCoNi)(70)Ti10B20. The amorphous alloy composition was confirmed by energy dispersive X-ray spectroscopy analysis that showed an excellent homogeneity of the alloying elements. The phase stability of the mechanically alloyed amorphous sample was further verified by employing high-temperature and high-pressure studies. The alloy samples heat-treated at 700 degrees C revealed crystallization of the amorphous phase. However, synchrotron-based high-pressure ambient temperature X-ray diffraction studies confirmed that the amorphous phase of the alloy remained stable up to the pressure of 30 GPa. The 50 h milled sample after being annealed at 350 degrees C showed improvement in the soft magnetic properties of the alloy, which was due to the probable elimination of the residual stress in the amorphous phase of the alloy powders. (C) 2020 Elsevier B.V. All rights reserved.Öğe Synthesis and characterization of amorphous-nanocrystalline Fe70Cr10Nb10B10 powders by mechanical alloying(Springer Heidelberg, 2022) Avar, Barış; Chattopadhyay, Arun K.; Şimşek, Tuncay; Şimşek, Telem; Özcan, Şadan; Kalkan, BoraIn this study, structural, morphological, thermal and magnetic properties of amorphous-nanocrystalline Fe70Cr10Nb10B10 (at.%) alloy are discussed. The formation and evaluation of amorphous-nanocrystalline structures of the alloy were followed by XRD, SEM-EDX, TEM, DTA, and VSM techniques. After 50 h of milling Cr, Nb, and B were completely dissolved into the Fe lattice forming 82% of the amorphous phase of the alloy. A gradual dissolution of the alloying elements also increased the lattice parameters concurrently. The lattice parameters reached a maximum value of 2.908 angstrom after 20 h of milling and then leveled off to a value of 2.891 angstrom at the end of 50 h of milling. Based on the XRD data, crystallite size and lattice strain of the alloy were calculated as 3.2 nm and 3.34% respectively. TEM analyses revealed that the alloy particulates comprised needle-shaped nanoparticles of an average size of 21 nm. The room temperature magnetic hysteresis loops showed that the increased duration of milling decreased the saturation magnetization from 91 to 24 emu/g. This was mainly due to the upsurge on the amorphous phase content in the alloy as the milling progressed. The increase in amorphous phase content and the subsequent reduction of the saturation magnetization were due to the inter-diffusion of the non-ferromagnetic Cr and B atoms into the Fe lattice. Thermal studies revealed that around 350 degrees C the amorphous phase of the alloy began crystallizing. The magnetic saturation of the heat-treated alloy also increased with the growth in the crystalline phases. The 50 h milled sample annealed at 700 degrees C was found to have the highest magnetic anisotropy as observed from the temperature-dependent zero-field cooled and field cooled magnetization measurements. The high-pressure X-ray diffraction measurements revealed that the amorphous state of the alloy remained stable up to 11.3 MPa. It also revealed the structural similarities of the Fe70Cr10Nb10B10 alloy with those of the Fe70M10B20 (M = Nb and Cr) types. For all practical purposes, the microstructural stability under high compressive pressure represents the consolidation properties of the nanostructured magnetic materials since both pressure and temperature-induced phase transformations are the primary controlling factors for the specific magnetization properties of the alloy.Öğe The effect of Cr and Nb addition on the structural, morphological, and magnetic properties of the mechanically alloyed high entropy FeCoNi alloys(Springer Heidelberg, 2022) Yakın, Alican; Şimşek, Telem; Avar, Barış; Chattopadhyay, Arun K.; Özcan, Şadan; Şimşek, TuncayIn this study, four different equimolar compositions of FeCoNi, FeCoNiNb, FeCoNiCr, and FeCoNiNbCr were synthesized by the mechanical alloying method. The effects of Cr and Nb addition on the structural, morphological, and magnetic properties of FeCoNi alloy were investigated in detail. The structural aspects of the samples were analyzed by X-ray diffractometer and scanning electron microscope equipped with an energy dispersive X-ray spectrometer. High and low-temperature magnetic properties were evaluated by a vibrating sample magnetometer. It was noticed that the addition of Nb caused amorphization, while Cr promoted crystallization in the alloys. The crystallite sizes were calculated as 9.7, 3.1, 8.3, and 4.4 nm for the FeCoNi, FeCoNiNb, FeCoNiCr, and FeCoNiCrNb alloys, respectively, after 20 h of milling. The SEM images of the as-milled alloys revealed irregular and layered structures for FeCoNi and FeCoNiCr alloys of mean particle sizes around 140 and 120 mu m. In contrast, the addition of Nb in these alloys, viz. FeCoNiNb and FeCoNiNbCr alloys, formed mostly spherical with irregular morphologies of particle sizes ranging between 55 and 80 mu m. It was noticed that the low solubility of Cr caused precipitation at the grain boundaries of the alloy particles, and it contributed to the formation of hard structures of irregular and layered morphologies. The observed increase in the lattice parameters and lattice strain in the solid solution phases of all-alloy systems studied was mainly due to the lattice distortion and intense plastic deformations. The maximum saturation magnetization obtained from the room temperature hysteresis loops was 150.4 emu/g for the FeCoNi alloy after 10 h of milling. The additions of non-magnetic Cr, Nb, and both into FeCoNi, caused a significant decrease in the saturation magnetization. The coercivity of the as-milled alloys was also found to decrease with the reduction in the nano-crystallite sizes, which elucidated that the crystallite sizes of the alloys were smaller than the magnetic exchange length. The high-temperature magnetization curves revealed that all alloys studied had Curie temperature higher than 700 K.
