Effect of Li doping on the critical temperature and glass formation in the Bi-Sr-Ca-Cu-O system

A study has been made of the glass-forming ability, structure, and superconducting properties of Bi_2.2Sr_1.8Ca_1.05Cu_2.15Li_xO_y and Bi_2.2Sr_1.8Ca_1.05Cu_2.15−x Li_xO_y (x=0;0.3;0.5;0.7). The compounds were melted by rf at T=1300–1500 °C. Rapid quenching produces glassy alloys whose glass-forming ability is the highest when lithium is substituted for copper. Glass annealing at 700–800 °C results in the formation of the HTSC phase 2212 with a critical temperature of up to 91 K. In lithium-doped samples the HTSC phase forms at lower temperatures and shorter anneals and it depends on the cooling rate following the anneal. The composition and properties of the 2212 phase depend nonmonotonically on the anneal time. The lattice parameter C of the 2212 phase increases with increasing lithium content. Fiz. Tverd. Tela (St. Petersburg) 41, 18–21 (January 1999)     

Production, structure, and microhardness of nanocrystalline Ni-Mo-B alloys

Radiography, differential scanning calorimetry, luminescence and high-resolution electron microscopy are used to study the production, nanocrystalline structure, stability, and microhardness of alloys from the Ni-Mo-B system containing from 27 at. % to 31.5 at. % Mo and 10 at. % B. All studies of these alloys indicated that annealing at 600 °C leads to the creation of a granular phase consisting of FCC nanocrystallites with average grain sizes of 15–25 nm, depending on the chemical composition of the alloy. Annealing these nanocrystalline samples isothermally at a temperature of 600 °C has no appreciable effect on the grain size. Structurally, the nanocrystalline phase consists of grains of an FCC solid solution of Mo and B in Ni, dispersed in an amorphous matrix that isolates them from one another. The lattice parameters of the FCC nanocrystallites depend on the alloy composition and the duration of their isothermal anneal. Within this latter time, molybdenum and boron atoms diffuse from the FCC solid-solution lattice into the surrounding amorphous matrix. The stability of the nanocrystalline structure is determined by the thermal stability of the amorphous matrix, whose crystallization temperature increases with the isothermal annealing time due to enrichment by boron and molybdenum. As the structure forms, the alloy becomes harder as the nanocrystalline grains grow in size. This relation between hardness and grain size, which is opposite to the Hall-Petch law, is explained by hardening of the amorphous matrix due to changes in its chemical composition. Fiz. Tverd. Tela (St. Petersburg) 40, 10–16 (January 1998)     

Chemical reduction of hematite by sodium borohydride

Well-crystallized hematite was suspended in water and treated at room-temperature (RT) with sodium borohydride. The product of the reaction is a highly magnetic black powder, which is stable at RT. The NaBH₄ treatment converts about half of the hematite to an amorphous Fe–B alloy and to a small fraction of sub-micron sized, amorphous metallic-Fe nodules. Heating at 400°C of this composite has resulted in the crystallization and/or oxidation of more than half of the amorphous Fe–B phase to α-Fe and Fe₃O₄ and B₂O₃, respectively. After treatment at 800°C, the metallic Fe and the amorphous Fe–B have completely vanished, and the resulting product consists of hematite and FeBO₃ embedded in the matrix of α-Fe₂O₃.     

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.     

Features of magnetic phase transitions in iron-manganese arsenides of the type Fe a−x MnxAs (a≈1.6)

This paper discusses how temperature/pressure processing affects the cascade of magnetic phase transitions in the alloy Fe_0.5Mn_1.1As with a C38 tetragonal crystal lattice. It shows that after various temperature/pressure treatment regimes (quenching of the sample from 800 °C under pressures of 30–60 kbar) no transition to the low-temperature phase is observed, as a result of which the ferrimagnetic phase extends to liquid-nitrogen temperatures. These results are analyzed on the basis of a qualitative model that takes into account the competition of ferromagnetic and antiferromagnetic interactions within and between nonequivalent crystallographic subsystems. Fiz. Tverd. Tela (St. Petersburg) 39, 889–893 (May 1997)     

Microstructural evolution and thermal stability of Fe–Zr metastable alloys developed by mechanical alloying followed by annealing

The effect of Zr (up to 1 at.%) addition on the formation of Fe–Zr metastable alloys and their thermal stability were investigated for their possible nuclear applications. Fe–xZr (x = 0.25, 0.5, 1%) alloys were synthesised by mechanical alloying under a high-purity argon atmosphere using stainless steel grinding media in a SPEX 8000M high energy mill. The milling was conducted for 20 h with a ball-to-powder weight ratio of 10:1. The formation of metastable solid solutions after milling was confirmed from the change in the Gibbs free energy analysis as per Miedema’s model. The microstructural characterisation was carried out by analysis of X-ray diffraction, atomic force microscopy and transmission electron microscopy. The effect of Zr on the thermal stability of Fe–Zr alloys was investigated by extensive annealing experiments followed by microstructural analysis and microhardness measurements. The stabilisation was found to occur at 800 °C and thereafter, no significant change in the crystallite size was observed for the samples annealed between 800 and 1200 °C. The supersaturated solid solution, especially 1% Zr alloy, found to be highly stable up to 800 °C and the microhardness value of the same measured to be as high as 8.8 GPa corresponding to a crystallite size of 57 nm. The stabilisation effect has been discussed in the light of both the thermodynamic and kinetic mechanisms and the grain size stabilisation is attributed to the grain boundary segregation of Zr atoms and/or Zener pinning by nanoscale precipitation of the Fe₂Zr phase.     

Observation of fine structure in the photoluminescence spectrum of an Er3+ ion in an amorphous silicon matrix

A multicomponent Stark structure corresponding to a 4I _13/2→4I _15/2 transition in the 4f ¹¹ shell of Er³⁺ ions is observed in hydrogenated amorphous silicon (a-Si:H) subjected to low-temperature (150 °C) anneal. The observation of narrow, strong components indicates that the erbium ions form a highly ordered local surrounding (Er-O-Si nanoclusters) in the labile, disordered structural network of a-Si:H. Pis’ma Zh. éksp. Teor. Fiz. 70, No. 12, 780–783 (25 December 1999) Deceased.     

Nanocrystallization of an amorphous Fe<Subscript>80</Subscript>B<Subscript>20</Subscript> alloy during severe plastic deformation

The structural evolution of an amorphous Fe₈₀B₂₀ alloy subjected to severe plastic deformation at room temperature or at 200°C was studied. Deformation leads to the formation of α-Fe nanocrystals in an amorphous phase. After room-temperature deformation, nanocrystals are localized in shear bands. After deformation at 200°C, the nanocrystal distribution over the alloy is more uniform. Possible causes of the crystallization of the amorphous phase during severe plastic deformation are discussed.     

Temperature dependence of amorphous and interface phases in the Fe80Nb7Cu1B12 nanocrystalline alloy

Temperature measurements (77–625 K) of Fe₈₀Nb₇Cu₁B₁₂ nanocrystalline alloy prepared from amorphous precursor annealed for 1 h at 470^°C and 620^°C are presented. Structural and magnetic behaviours of the crystalline phase, the amorphous residual matrix, and the interface zone between crystalline grains and the amorphous phase are studied by distributions of hyperfine magnetic fields. Magnetic regions are developing in the retained amorphous phase with rising temperature of annealing. They can be suppressed, however, at high enough measuring temperatures turning the amorphous matrix into paramagnetic state. As a consequence, the respective spectral components do not interfere so much and the role of interface zone can be studied. This revised version was published online in July 2006 with corrections to the Cover Date.     

Structural evolutions of the mechanically alloyed Al<Subscript>70</Subscript>Cu<Subscript>20</Subscript>Fe<Subscript>10</Subscript> powders

Elemental mixtures of Al, Cu, Fe powders with the nominal composition of Al₇₀Cu₂₀Fe₁₀ were mechanically alloyed in a planetary ball mill for 80 h. Subsequent annealing of the as-milled powders were performed at 600–800°C temperature range for 4 h. Structural characteristics of the mechanically alloyed Al₇₀Cu₂₀Fe₁₀ powders with the milling time and the heat treatment were investigated by X-ray diffraction (XRD), differential scanning calorimeter (DSC) and differential thermal analysis (DTA). Mechanical alloying of the Al₇₀Cu₂₀Fe₁₀ did not result in the formation of icosahedral quasicrystalline phase (i-phase) and a long time milling resulted in the formation of β-Al(Cu,Fe) solid solution phase (β-phase). The i-phase was observed only for short-time milled powders after heat treatment above 600°C. The β-phase was one of the major phases in the Al₇₀Cu₂₀Fe₁₀ alloy. The w-Al₇Cu₂Fe₁ phase (w-phase) was obtained only after heat treatment of the short-time milled and unmilled samples. The present investigation indicated that a suitable technique to obtain a large amount of quasicrystalline powders is to use a combination of short-time milling and subsequent annealing.     

Exciton luminescence of Cd1−x FexTe solid solutions

Band-edge optical spectra of Cd_1−x Fe_xTe solid solutions differ substantially from those of undoped CdTe. The pattern of the change in photoluminescence spectra with increasing Fe concentration is connected with a change in radiative recombination channels. Fiz. Tverd. Tela (St. Petersburg) 40, 897–899 (May 1998)     

Effect of temperature on the magnetoimpedance of an elastically deformed Fe<Subscript>4</Subscript>CO<Subscript>67</Subscript>Mo<Subscript>1.5</Subscript>Si<Subscript>16.5</Subscript>B<Subscript>11</Subscript> foil

The effect of temperature and elastic tensile stresses on the magnetoimpedance of an amorphous Vitrovac 6025Z (Fe₄CO₆₇Mo_1.5Si_16.5B₁₁) foil is studied. Two temperature ranges (20–70 and 70–220°C) in which the effect of elastic tensile stresses on the magnetoimpedance has different characters are detected. The existence of these two temperature ranges is shown to be caused by a change in the sign of a magnetostriction constant at 70°C.     

Electronic and topological parameters of the skin layer in amorphous metallic ribbons after thermal annealing

Data on spectral polarimetric measurements in the range of 0.05–0.60 eV are presented, along with calculations on the optical characteristics of the surface layers of ribbons of the amorphous alloy Co₅₉Fe₅Ni₁₀Si₁₁B₁₅ before and after thermal annealing in order to determine how the composition of the surface layer changes during this treatment. It is shown that after annealing at a temperature of 425°C or above, the optical conductivity and the real and imaginary parts of the dielectric constant revert to the values for typical metals in the IR. This treatment produces microregions with an ordered structure in the surface layer. The experimental data show that for ribbons annealed at T = 475°C the spectral optical characteristics do not obey the Drude relations and behave similarly to their amorphous analogs.     

Low temperature annealing of ball-milled Fe66B34

High energy ball-milling of Fe and B powders of starting composition Fe₆₆B₃₄ resulted in an alloy which revealed both a nanostructural state and a disordered amorphous-like state and a majority of unreacted components. The disordered phase is located in the interfacial regions between the Fe and B atoms. The ball-milled sample was annealed at low temperatures (250–350°C) to examine further the proposition that solid-state reaction is the mechanism of amorphization by mechanical alloying. A slight reaction between the Fe and B grains which were previously unreacted, probably limited to their contacting boundaries, has been detected.     

Temperature dependence of the magnetic properties and magnetoimpedance of nanocrystalline Fe<Subscript>73.5</Subscript>Si<Subscript>16.5</Subscript>B<Subscript>6</Subscript>Nb<Subscript>3</Subscript>Cu<Subscript>1</Subscript> ribbons

The temperature dependences of the magnetic properties and the magnetoimpedance effect of soft magnetic nanocrystalline Fe_73.5Si_16.5B₆Nb₃Cu₁ alloy ribbons are studied in the temperature range 24–160°C. A high temperature sensitivity of the impedance and the magnetoimpedance effect of the ribbons are detected in the ac frequency range 0.1–50 MHz. At an ac frequency of 50 MHz, the change in the impedance reaches 0.2 Ω/°C (0.5%/°C) in the temperature range 85–160°C. When the temperature increases, a monotonically decreasing character of the dependence of the magnetoimpedance effect on the applied magnetic field changes into a dependence having an increasing initial segment. The effect of temperature on the magnetoimpedance properties of the soft magnetic nanocrystalline ribbons is shown to result from temperature-induced changes in their electrical conductivity, magnetization, and effective magnetic anisotropy.     

Mössbauer study of Fe-B alloys containing Nd additives

The influence of a few percent neodynium additives to Fe-B alloy on the hyperfine parameters was investigated. It was found that Nd decreases the hyperfine field of amorphous Fe-B alloys. The samples annealed at temperatures between 600°C and 700°C contain α-Fe and Fe₃B phases. The average hyperfine field of Fe₃B phase increases with increasing Nd content and decreases with increasing annealing temperature. The average isomer shift of Fe₃B phase decreases with increasing Nd content. The experimental data show that the change of hyperfine parameters of the Fe₃B phase in the studied alloys is due to Nd atom.     

Kinetics of ß-phase transformation in the heat treatment of FeSi2- and Fe2Si5-based thermoelectric alloys

FeSi₂- and Fe₂Si₅-based thermoelectric alloys have been fabricated by melt spinning and levitation melting. It was found that the levitation-melted FeSi₂-based alloy must be annealed at 800°C for 10 h to complete transformation of the β phase, while an anneal for only 6 h was needed for the melt-spun alloy. On the other hand, annealing the levitation-melted Fe₂Si₅-based alloy for 4 h was enough to complete β-phase formation, whereas 14 h was required for the melt-spun alloy. Annealing temperature dependence of the Seebeck coefficient showed that the maximum rate of transformation to β phase occurred at about 800°C for all samples. Application of the Johnson-Mehl-Avrami equation revealed that grain-boundary nucleation was predominant in the levitation-melted FeSi₂-based alloy (time exponent n = 1.1), while the zero nucleation mechanism was operative in the melt-spun alloy (n = 3.1). For the eutectoid reactions in the Fe₂Si₅-based alloys, several kinds of nucleation site were active. However, nuclei formed at grain edges were dominant in the melt-spun alloy since n = 1.6.     

Colossal magnetoresistance of FexMn1−xS magnetic semiconductors

The magnetic, electric, magnetoresistive, and structural properties are investigated in the sulfide solid solutions Fe_xMn_1−2x S, which are based on the antiferromagnetic semiconductor α-MnS (the fcc NaCl lattice). Colossal negative magnetoresistance (δ_H∼−83% at 160 K for x ∼ 0.29), comparable to that observed in La-Ca-Mn-O polycrystals and films (δ_H∼−90% at 100 K and 40 kOe), is observed in compounds with intermediate concentrations 0.26<x<0.4, corresponding to the region of incipient ferromagnetism. Pis’ma Zh. éksp. Teor. Fiz. 69, No. 12, 895–899 (25 June 1999)     

Domain structure fluctuations kinetics of amorphous alloys at low-temperature annealing

Previously reported spin orientation fluctuations of the amorphous Fe₈₁B₁₉ alloy at temperatures well below the onset of crystallization were directly shown by the time scanning experiment at 250 °C. The connection of this effect with the magnetostriction field and α-Fe nuclei at the contact surface was proved by the CEMS spectra and by vanishing the effect at both the etched-off Fe₈₁B₁₉ and a zero magnetostriction samples.     

Influence of synthesis method on structural and magnetic properties of cobalt ferrite nanoparticles

The Co–ferrite nanoparticles having a relatively uniform size distribution around 8 nm were synthesized by three different methods. A simple co-precipitation from aqueous solutions and a co-precipitation in an environment of microemulsions are low temperature methods (50 °C), whereas a thermal decomposition of organo-metallic complexes was performed at elevated temperature of 290 °C. The X-ray diffractometry (XRD) showed spinel structure, and the high-resolution transmission electron microscopy (HRTEM) a good crystallinity of all the nanoparticles. Energy-dispersive X-ray spectroscopy (EDS) showed the composition close to stoichiometric (~CoFe₂O₄) for both co-precipitated nanoparticles, whereas the nanoparticles prepared by the thermal decomposition were Co-deficient (~Co_0.6Fe_2.4O₄). The X-ray absorption near-edge structure (XANES) analysis showed Co valence of 2+ in all the samples, Fe valence 3+ in both co-precipitated samples, but average Fe valence of 2.7+ in the sample synthesized by thermal decomposition. The variations in cation distribution within the spinel lattice were observed by structural refinement of X-ray absorption fine structure (EXAFS). Like the bulk CoFe₂O₄, the nanoparticles synthesized at elevated temperature using thermal decomposition displayed inverse spinel structure with the Co ions occupying predominantly octahedral lattice sites, whereas co-precipitated samples showed considerable proportion of cobalt ions occupying tetrahedral sites (nearly 1/3 for the nanoparticles synthesized by co-precipitation from aqueous solutions and almost 1/4 for the nanoparticles synthesized in microemulsions). Magnetic measurements performed at room temperature and at 10 K were in good agreement with the nanoparticles’ composition and the cation distribution in their structure. The presented study clearly shows that the distribution of the cations within the spinel lattice of the ferrite nanoparticles, and consequently their magnetic properties are strongly affected by the synthesis method used.