Synthesis and magnetic properties of Laves phase Fe<Subscript>2</Subscript>Nb amorphous alloy

The formation process and magnetic properties of the Laves phase compound of nominal composition Fe₂Nb in its amorphous phase prepared by mechanical alloying have been investigated. The effect of milling time on the formation of amorphous phase has been studied using an X-ray diffraction technique. Further characterizations were carried out by particle size measurement, dc magnetization, ac susceptibility and ferromagnetic resonance studies. Magnetization and susceptibility studies show soft ferromagnetic behaviour, whereas ferromagnetic resonance studies show some sort of disorder/strain introduced during the mechanical alloying process. PACS 74.70.Ad; 61.82.Bg; 74.25.Ha; 75.60.Ej; 76.50.+g     

Formation and magnetic properties of mechanically alloyed Al65Cu20Fe15 quasicrystal

The formation of icosahedral phase by mechanical alloying of crystalline elemental powder of Al, Cu and Fe has been investigated. The effect of milling time on the formation of icosahedral phase of nominal composition of Al₆₅Cu₂₀Fe₁₅ has been studied using the X-ray diffraction technique. Further studies have been carried out by scanning electron microscopy (SEM), energy-dispersive X-ray microanalysis (EDAX), particle size, magnetisation and ferromagnetic resonance studies. All these studies indicate that the icosahedral alloy shows soft ferromagnetic behaviour.     

Mössbauer, X-ray diffraction and magnetization studies of Fe–Mn–Al–Nb alloys prepared by high energy ball milling

Fe₆₀Mn₁₀Al₂₀Nb₁₀, (Fe₆₀Mn₁₀Al₃₀)₉₅Nb₅ and (Fe₆₀Mn₁₀Al₃₀)₉₀Nb₁₀ ball milled powdered alloys were investigated using X-ray diffraction, Mössbauer spectrometry, thermomagnetic (TGM) and magnetization measurements. We studied the influence of Nb content and of different milling times on the structural and magnetic properties. Two main features can be concluded: (1) the FeAlMn induces a BCC phase whatever the Nb content is, and (2) as both increasing Nb content and milling time give rise to an highly disordered state in conjunction with a decrease of the ferromagnetic behavior.     

Formation of Fe-Nb-X (X=Zr, Ti) amorphous alloys from pure metal elements by mechanical alloying

Fe-based amorphous powders of Fe₅₆Nb₆Zr₃₈ and Fe₆₀Nb₆Ti₃₄ based on binary eutectic were prepared by mechanical alloying starting from mixtures of pure metal powders. The amorphization behavior and thermal stability were examined by x-ray diffraction, scanning electron microscopy, transmission electron microscopy and differential scanning calorimetry. Results show that Fe₅₆Nb₆Zr₃₈ alloy has a better glass forming ability and a relatively lower thermal stability comparing with Fe₆₀Nb₆Ti₃₄ alloy. The prepared amorphous powders have homogeneous element distribution and no obvious contaminants coming from mechanical alloying. The synthesized amorphous powders offer the potential for consolidation to full density with desirable mechanical properties through the powder metallurgy methods.     

Magnetic properties of the mechanically alloyed Fe0.9-xMn0.1Alx system

Samples of nominal composition Fe_0.9-xMn_0.1Al_x (0.1 ? x ? 0.5) were prepared by mechanical alloying starting from pure elements. Milling times of 24, 72 and 144 h were considered. The magnetic properties of the samples were studied by using ⁵⁷Fe Mössbauer spectroscopy, vibrating sample magnetometry and magnetic susceptibility measurements. The phase distribution was determined from X-ray diffractometry. The so obtained results evidence a strong dependence on the milling time and Al concentration of the room-temperature hyperfine field distributions and coercive forces. The susceptibility measurements in the range of temperature between 10 K and 180 K suggest the occurrence of different types of transitions as the temperature is increased: (a) from a ferromagnetic to a paramagnetic phase, (b) from a reentrant spin-glass phase to a ferromagnetic one and (c) from spin-glass to a paramagnetic phase. These transitions are also strongly influenced by the milling time and the Al concentration.     

Influence of demagnetization effect on giant magneto-impedance of soft ferromagnetic metal

The magneto-impedance (MI) of an amorphous ferromagnetic ribbon with nominal composition Fe₄₀Ni₄₀B₂₀ and of different lengths is measured using non-contact method at 1 MHz frequency. In the presence of static magnetic field around 30 Oe, the MI of the ribbon of long length is reduced by nearly 90%. With decreasing sample dimension the extent of reduction in MI becomes smaller. The MI of a ferromagnetic metallic system results from the e.m field’s screening which in turn depends on the magnetic response of the sample. The demagnetization field of smaller sample size reduces the magnetic response which in turn decreases the field sensitivity of MI. The phenomenology based on the Landau–Gilbert equation predicts similar qualitative behaviour of MI.     

A Comparative Study on the Magnetic Properties of Arc-Melted and Ball-Milled Fe0.9−x Mn0.1Al x Alloys

Samples of nominal composition Fe_0.9?x Mn_0.1Al _x (0.1 ≤x≤0.5) were prepared both by mechanical alloying and arc-melting. In order to elucidate the effect of the synthesis method upon the magnetic properties of this system, we have carried out a comparative study involving the use of different experimental techniques (Mössbauer, X-ray diffraction, vibrating sample magnetometry and magnetic susceptibility). Results revealed that independently of the employed method and milling time, the samples exhibit ferromagnetism below ～34 at.% Al. Above this concentration, the preparation method became a determinant factor upon the magnetic properties of the system. The differences are attributed, in the case of the mechanically alloyed samples, to Fe contamination arising from jars material. The results of our study are summarized in a magnetic phase diagram including ferromagnetic, paramagnetic, pure spin glass and reentrant spin glass regions.     

The effect of thermal treatment on the magnetic properties of Ge-doped FeNbB alloys

The effects of Ge doping on the magnetic properties of nanocrystalline FeNbB ribbons are investigated. For amorphous Fe₈₀Nb₁₀Ge₃B₇ alloy, three crystallization processes are observed when heated from room temperature to 1173 K. At 973 K, a harder magnetic phase is formed, which brings about a constricted hysteresis loop. A large increase of relaxation frequency and a dramatic drop of permeability of 973 K-annealed Fe₈₀Nb₁₀Ge₃B₇ alloy are observed. The presence of Nb is essential for the nanocrystallization of α-Fe grains. If Nb is replaced by Ge completely, the thermal treatment will lead to the formation of coarse-grained Fe₃Ge phase rather than nanosized α-Fe grains. The coarse-grained Fe₃Ge results in a remarkable drop in magnetic softness. PACS 75.75.+a; 75.50.Bb     

Characterization of phases in the Fe-Nb system

The Fe-Nb system was investigated by means of X-ray diffraction and Mössbauer spectroscopy (at 300 and 77 K), in the range from 1 to 66.7 at%. We have found that the limit of solubility of Fe in Nb at 1100°C is between 3 and 4 at% Fe, and observed the coexistence of the Nb solid solution (Nbss) phase and Fe₂₁Nb₁₉ in the range from 4 to 40 at% Fe. The Mössbauer parameters of all the single phases are reported. The lattice parameters of Nbss phase present no significant variation with the Nb content. The X-ray pattern for the Fe₂₁Nb₁₉ phase could not be solved. The Laves phase Fe₂Nb presents Mössbauer and X-ray parameters that agree with the literature.     

Nb(Ba)加强Bi系中2223相生成作用研究

固相法合成系列名义组成为Bi_2-xNb_xSr₂Ca₂Cu₃O_y(x=0—1.0)的样品,电学和磁学测量表明,当掺入x=0.2—0.3的Nb有明显加强2223相生成的作用,配比为Bi_1.7Nb_0.3Sr₂Ca₂Cu₃O_y时最佳;当掺Ba以部分取代Sr后有明显协同Nb促进2223相生成的作用,比单掺Nb效果更为显著,其中以Bi_1.7Nb_0.3Sr_1.8Ba_0.2Ca₂Cu₃O_y为最优组成。热重分析(TGA)实验显示,掺Nb(Ba)后样品在～600°C出现吸氧增重;XPS中的O_1s峰显示掺Nb(Ba)后除～531eV的主峰外,在～529eV的肩峰更加明显;讨论了Nb(Ba)对晶体结构的可能影响。 关键词：     

Structural, thermal and optical studies of mechanical alloyed Ga40Se60 mixture

A mixture of elemental Ga and Se with the nominal composition Ga₄₀Se₆₀ was submitted to the Mechanical alloying technique and their structural, thermal and optical properties were followed by X-ray diffraction, differential thermal analysis, photoacoustic spectroscopy, UV-VIS‐NIR absorbance spectroscopy and Raman spectroscopy techniques. After 10 h of milling the X-ray pattern showed monoclinic Ga₂Se₃ phase nucleation, which is in the nanometric form, and also a minority amorphous phase. The DSC results showed exothermic reactions between 430 and 720 K attributed to amorphous-crystalline phase transition and structural relaxation of Ga₂Se₃ phase. Based on this a small amount of the as-milled sample was annealed at 723 K. Its XRD pattern showed evidences of grain growth, reduction of the interfacial component, as well as, disappearance of the amorphous phase. The annealing process induced thermal diffusivity increasing, while the optical band gap energy and Raman profile remained practically unchanged.     

Structural relaxation,crystallization and improvement of magnetic properties in FeXSiB (X=Cr,Nb)-type amorphous alloys

In the present paper, the influence of Nb and Cr on intensity of structural relaxation, crystallization processes, electric and magnetic properties in the Fe₇₆Nb₂Si₁₃B₉, Fe₇₆Cr₂Si₁₃B₉ and Fe₇₆Nb₁Cr₁Si₁₃B₉ alloys were investigated. It was shown that the improvement of magnetic permeability caused by a suitable annealing is a thermally activated process. Activation energy of this process is found to be of the order of 1 eV. Cr as an alloying addition to the Fe–Si–B alloy does not change the 1 h optimization annealing temperature and causes an increase of its efficiency. Nb as an alloying addition causes an increase of the 1 h optimization annealing temperature, and also the temperature of the first step of crystallization.     

Mössbauer study of intergranular phase in Nd 8 Fe86 − x Nb x B6(x = 0, 1, 2, 3) nanocomposite magnet

Nd₈Fe_86???x Nb _x B₆ (x = 0, 1, 2, 3) nanocomposite magnet has been studied by Mössbauer spectroscopy and nanostructure observation. It was found that intergranular phase formed between α-Fe and Nd₂Fe₁₄B phase in NdFeNbB alloys plays a significant role on the magnetic properties. By the addition of Nb into Nd₈Fe₈₆B₆ composition, coercivity was found to increase by 25% due to the grain refinement of both the soft and hard magnetic phases which was decreased from 50 nm of virgin Nd₈Fe₈₆B₆ to 25 nm in Nd₈Fe₈₅Nb₁B₆ alloys. The role of Nb addition was confirmed to stabilize the Nd₂Fe₁₄B lattice preventing from thermal vibration of the corresponding sites at where Fe atoms are substituted by Nb in the Nd₂Fe₁₄B lattice. The enhanced coercivity was originated from the exchange hardening of soft and amorphous phases surrounding the hard magnetic Nd₂Fe₁₄B crystal.     

Magnetic and structural properties of mechanically alloyed Tb0.257−x Nd x Fe0.743 alloys, with x = 0 and 0.257

The alloys between a transition metal and a rare earth present magnetic and magneto optical properties of exceptional interest for the production of magnetic devices for information storage. In this work we report the magnetic and structural properties, obtained by Mössbauer spectrometry (MS) and X-ray diffraction (XRD), of Tb_0.257?x Nd _x Fe_0.743 alloys with x?=?0 and 0.257 prepared by mechanical alloying during 12, 24 and 48 h, to study the influence of the milling time in their magnetic and structural properties. The X-rays results show for all the samples that the α-Fe and an amorphous phase are always present. The first decreases and the second increases with the increase of the milling time. Mössbauer results show that the amorphous phase in samples with Nd is ferromagnetic and appears as a hyperfine field distribution and a broad doublet, and that as the milling time increases the paramagnetic contribution increases. For samples with Tb the amorphous phase is paramagnetic and appears as a broad doublet which increases with the milling time and for 48 h milling it appears an additional broad singlet.     

Nanocrystalline Fe/Zr alloys: preparation by using mechanical alloying and mechanical milling processes

Nanocrystalline Fe/Zr alloys have been prepared after milling for 9 h the mixture of elemental Fe and Zr powders or the arc-melting produced Fe₂Zr alloy by using mechanical alloying and mechanical milling techniques, respectively. X-ray and Mössbauer results of the Fe and Zr powders, mechanically alloyed, suggest that amorphous Fe₂Zr phase and $\upalpha$ -Fe(Zr) nanograins have been produced with relative concentrations of 91% and 9%, respectively. Conversely, the results of the mechanically milled Fe₂Zr alloy indicate that nanograins of the Fe₂Zr alloy have been formed, surrounded by a magnetic inter-granular phase that are simultaneously dispersed in a paramagnetic amorphous phase.     

FINEMET type alloy without Si: Structural and magnetic properties

Magnetic and structural properties of a Finemet type alloy (Fe_73.5Ge_15.5Nb₃B₇Cu₁) without Si and high Ge content were studied. Amorphous material was obtained by the melt spinning technique and was heat treated at different temperatures for 1 h under high vacuum to induce the nanocrystallization of the sample. The softest magnetic properties were obtained between 673 and 873 K. The role of Ge on the ferromagnetic paramagnetic transition of the as-quenched alloys and its influence on the crystallization process were studied using a calorimetric technique. Mössbauer spectroscopy was employed in the nanocrystallized alloy annealed at 823 K to obtain the composition of the nanocrystals and the amorphous phase fraction. Using this data and magnetic measurements of the as-quenched alloy, the magnetic contribution of nanocrystals to the alloy annealed at 823 K was estimated via a linear model.     

Crystallisation kinetics of amorphous Fe72.5−xCu1Nb4.5Si10+x+y B12-y alloy

Fe_73.5Cu₁Nb₃Si_13.5B₉ and Fe_72.5–xCu₁Nb_4.5Si_10+x+y B_12–y alloys are compared from the point of view of crystallisation behaviour and changes in the short-range order in the amorphous reminder. The increase in Nb to 4.5 at.% in the latter system slows down the formation of nanocrystals to approximately 40% even after 16 hours of anneal at 550 °C forx=0.5,y=3. Segregation-induced changes in the short-range order are manifested via hyperfine field distributions corresponding to the amorphous reminder.     

Studies of the relaxed amorphous phase in the Fe80Nb6B14 alloy

The paper presents measurements of magnetic permeability, magnetic after-effects, magnetostriction, DSC and XPS for the Fe₈₀Nb₆B₁₄ amorphous alloys preliminary annealed for 1 h at temperatures ranging from 300 to 770 K. It was shown that annealing out of free volume and internal stresses causes a decrease of magnetostriction coefficient and leads to the formation of the energetically stable relaxed amorphous state. The XPS spectra show local fluctuation of boron density. This effect was attributed to the formation of small iron clusters—the characteristic feature for the relaxed amorphous phase.     

Ball milling of Fe40Ni40P20-xSix (x = 6, 10 and 14): production and characterization

Progress in the ball milling amorphization of elemental powders with the overall composition Fe₄₀Ni₄₀P_{20 ? x}Si_x (X = 6, 10 and 14) and thermally induced crystallization of obtained alloys were characterized by differential scanning calorimetry, X-ray diffraction and transmission Mössbauer spectroscopy (TMS). Diffusion of Si into Fe and Ni alloys promotes the formation of the amorphous phase, via previous formation of (Fe, Ni) phosphides. After milling for 32–64 h, most of the powders are amorphous but bcc Fe(Si) crystallites remain (about 5% in volume). TMS results indicate that homogenization of the amorphous phase occurs by interdiffusion of Ni and Fe in Fe(Si,P)-rich and Ni(Si,P)-rich zones respectively. Annealing induces structural relaxation of stresses induced by milling, growth of bcc Fe(Si) crystallites, precipitation of bcc Fe(Si) and fcc Ni–Fe, and minor phases of Ni-rich silicides and (Fe, Ni) phosphides. The main ferromagnetic phase is bcc Fe(Si) for Fe₄₀Ni₄₀P₁₀Si₁₀ powders obtained after milling for 32 h. However, it is fcc Fe–Ni for the same alloy after milling for 64 h. In the later powders, as well as for alloys with x = 6 and 14 milled for 32 h, the fcc Fe–Ni shows the Invar magnetic collapse.     

Effect of niobium on microstructure and magnetic properties of bulk anisotropic NdFeB/α-Fe nanocomposites

Bulk anisotropic NdFeB/α-Fe nano-composites were obtained directly from alloys of Nd₁₁Dy_0.5Fe_82.4−xNb_xB_6.1 (x=0,0.5,1.0,1.5). High resolution transmission electron microscopy images showed the existence of Nb-rich amorphous grain boundary phase in the alloys with Nb doped. Field emission scanning electron microscope morphologies and X-ray diffraction patterns revealed the grain size and grain alignment of hot pressed and hot deformed nanocomposites. It was found that Nb could refine the grain size and grain texture in hot worked ribbons. Vibrating sample magnetometer results showed that the magnetic properties of the anisotropic nanocomposites were improved with increased Nb doping. The remanence, coercivity and maximum energy product of the bulk anisotropic Nd₁₁Dy_0.5Fe_80.4Nb₂B_6.1 nanocomposites were 1.04 T, 563 kA/m and 146 kJ/m³, respectively.