Phase diagram of SrSi2 to 40 kbar and 1200°C

The pressure-temperature phase diagram of dimorphic SrSi₂ was investigated in the pressure range 10–40 kbar and temperature range 600–1200°C in a belt-type apparatus. The phase boundary between cubic SrSi₂I (SrSi₂-type) and tetragonal SrSi₂II (-ThSi₂-type) was studied by X-ray techniques in quenched samples. The curvature of the equilibrium line was not resolved. Molar volumes of both polymorphs have been measured in the temperature range 20–400°C at ambient pressure. From the slope of the equilibrium line in the pressure-temperature diagram and the change in molar volume, approximate values of the entropy and heat of transition SrSi₂(I–II) have been calculated.

In the silicon sublattice of both polymorphs of SrSi₂ the topologically simplest three-dimensional three-connected nets are found to be slightly distorted from their ideal configurations. The ideal SrSi₂-type net represents the three-connected analogy to the four-connected diamond net.     

Laser surface alloying of pure titanium with TiN–B–Si–Ni mixed powders

Laser alloying was carried out on the surface of pure titanium substrate with TiN–B–Si–Ni mixed powders. The result of X-ray diffraction (XRD) analysis shows that the alloyed layer consists of many kinds of intermetallic compounds. The test results show that the alloyed layers have high microhardness (1500–1600 HV_0.1), low friction coefficient (about 0.4), and are more resistant to oxidation than untreated substrate.     

Neutron diffraction and IR spectroscopy on mechanically alloyed La-substituted PbWO4

Defect structures of the lanthanum-substituted PbWO₄ prepared by mechanical alloying (MA) were investigated by means of powder neutron diffraction and FT-IR, to compare with that of the oxide ion conductive sintered samples. Neutron diffraction revealed that Pb_1−xLa_xWO_4+x/2 prepared by MA possessed the lead site deficiency in the lattice. In addition, it was also found that occupation factors of the lead site were still smaller than the nominal value even for the mechanically alloyed Pb_1−xLa_2x/3WO₄. The vacancy formation at the lead site of the mechanically alloyed Pb_1−xLa_xWO_4+x/2 was also corroborated from the splitting of the absorption band around 800 cm⁻¹ ascribed to the W–O stretching vibration of WO₄ tetrahedron. At the end of this paper, the formation process of the lead site vacancy was discussed in the sintered Pb_1−xLa_xWO_4+x/2 during milling.     

Coexisting antiferromagnetism and ferromagnetism in mechanically alloyed Fe-rich Fe–Ni alloys: implications regarding the Fe–Ni phase diagram below 400°C

Fe–Ni alloys below the Invar region with compositions Fe_100−xNi_x (x=21, 24, and 27 at%) were prepared by high-energy ball milling technique (mechanical alloying). The as-milled samples, characterized by X-ray diffraction and Mössbauer spectroscopy, contain a mixture of (BCC) and γ (FCC) phases, whereas the samples annealed at 650°C for 0.5 h show a single γ (FCC) phase displaying a single line Mössbauer spectrum at room temperature (RT). At low temperature, the Mössbauer spectra of annealed Fe₇₆Ni₂₄ and Fe₇₃Ni₂₇ alloys show the existence of a magnetically split pattern together with a broad singlet, which are ascribed to a high-moment ferromagnetic Ni-rich phase and a low-moment Fe-rich phase, respectively. The Fe-rich phase in annealed Fe₇₆Ni₂₄ alloy, which is paramagnetic at RT, undergoes antiferromagnetic ordering at 40 K, estimated from the dramatic line broadening of its spectrum, giving rise to a small hyperfine field (e.g. 2 T at 6 K). The coexistence of these phases is attributed to phase segregation occurring in these alloys as a result of enhanced atomic diffusion. The stability of these alloys towards martensitic (FCC→BCC) transformation at low temperatures is discussed in connection with the Fe–Ni phase diagram below 400°C.     

Investigation of magnetic, thermal and hyperfine properties of Tb in tetragonal sites in SrF2

The crystalline Stark splitting of the electronic ground state and various properties of Tb³⁺ in tetragonal sites in Tb: SrF₂ have been determined with the crystal field parameters of Antipin et al. Two singlets are found to lie lowest, the separation between them being 0.363 cm⁻¹. The χ has a Curie type variation in the range 4–1.0 K below which saturation effects set in. χ has a maximum at 110 K and becomes nearly temperature independent at around 4 K. The magnetic moment turns out to be 9.58 at 300 K which is very close to the free ion value 9.72. There is only a small variation of the magnetic moment with temperature. Two anomalies are found to occur in the Schottky heat capacity curve, one at 100 K, and the other at 0.22 K. The magnetic hyperfine field at the nucleus of Tb³⁺ is obtained as 3.456 MG, neglecting the core polarization. The temperature averaged electric quadrupole splitting of the nuclear ground state of ¹⁵⁹Tb has been calculated at different temperatures and is found to rise smoothly with the decrease of temperature to attain saturation at 10 K. The behavior of the hyperfine heat capacity C_N has been studied theoretically in the range 4.2–0.01 K. A Schottky anomaly appears at 0.1 K. The computations have been carried out in the intermediate coupling approximation.     

Mechanical and thermodynamic properties of infrared transparent low melting chalcogenide glass

The properties of infrared (IR) transparent chalcogenide glass Se₅₇I₂₀As₁₈Te₃Sb₂ have been studied for the first time by dynamic mechanical analysis (DMA). This glass demonstrates both high transparency in a broad IR band (1–12 μm) and a particularly low softening point (near 50 °C). It is known as one of the best adhesives intended for the binding of IR optics elements. The DMA method gives valuable information about the complex Young’s modulus of the glass in its softening region. In parallel with the study of mechanical properties of the glass the character of its glass transition process has been investigated. Our results of DMA were then compared with our thermodynamic data obtained by scanning calorimetry. The peak of mechanical losses in DMA appears to be situated considerably higher than the calorimetrically determined glass transition temperature.     

Magnetic properties of mechanically alloyed Co–Ti powder

An amorphous phase containing traces of non-transformed Co and Ti powders was obtained by mechanical alloying nominal compositions of Co₆₇Ti₃₃ and Co₅₀Ti₅₀ in a high-energy ball-mill. These alloys were prepared from elemental powders of Co and Ti. The heat treatment of Co₆₇Ti₃₃ at 573, 873 and 1173 K crystallized nanoparticles of Co₂Ti and Co₃Ti compounds, while the same treatments conducted on Co₅₀Ti₅₀ resulted in the formation of Co₂Ti and CoTi nanoparticles. The saturation magnetizations reached a maximum value in the amorphous state and they decreased when the temperatures of the heat treatment rose. Demagnetizing interparticle interaction effects were estimated through hysteresis loops and initial magnetization curves using the Fourier technique.     

Effects of composition and processing on properties of modified maghemite for high-density recording

The effects of composition and processing on the magnetic properties of Co, Mn and Zn modified maghemite particulates obtained by coprecipitation from aqueous solutions and heat treatment have been explored. It was found that the saturation (at 2 T) magnetization, of 63–75 emu/g and residual magnetization of 45–52 emu/g change little with the composition studied (6–14.4 wt% Mn and 8–15 wt% Co), while coercivity (1100–2200 Oe) does. The temperature coefficient of coercivity (TCC) was -0.24 to -0.39%/°C, depending only on composition. The Co content was found to dominate coercivity, while Mn led to a better heat treatment response of the particulates. Low-level Zn doping enhanced magnetization and reduced the TCC.     

Phase relationships in an Al3 (Ti,V) based in-situ composite

The phases and the crystallographic relationships between phases observed in an Al₇₀Ti₁₀V₂₀ alloy following chill casting and post-solidification heat treatment have been characterized using analytical transmission electron microscopy and electron diffraction. The chill-cast microstructure comprised a mixture of primary dendrites of δ-Al₃ (Ti,V) and interdendritic eutectic zones in which the continuous phase was δ-Al₃ (Ti,V) and the rode-like discontinuous phase was ζ-Al₈V₅. Following isothermal heat treatments in the temperature range 1073–1273 K, a uniform distribution of rod-like particles was observed to develop throughout the δ matrix and a phase transformation was detected within the dispersed particles, as the intermetallic ζ phase was replaced by b.c.c.β-(Ti,V) metallic solid solution. This transformation was typically complete within 100 hr at 1073 K, leading to the formation of an in-situ composite consisting of a uniform dispersion of metallic β-phase in a brittle Al₃(Ti,V) intermetallic matrix. The orientation relationship between the discontinuous β-(Ti,V) particles and the DO₂₂δ-Al₃(Ti,V) matrix involved parallelism of the closest-packed planes and close-packed directions in those planes, i.e. (110)_β//(112)_δ(DO22) and [ 11]_β//[ 10]_δ(DO22).     

Kinetic aspects of aluminium titanate layer formation on titanium alloys by plasma electrolytic oxidation

The paper reports on a systematic investigation into the effects of process parameters on the growth kinetics and associated changes in the structure, phase composition and mechanical properties of surface layers formed on Ti–6Al–4V alloy by plasma electrolytic oxidation (PEO) treatment in 0.05–0.2 mol l⁻¹ solutions of sodium aluminate. Methods of gravimetric, SEM and XRD analysis, as well as microhardness and scratch testing, are employed to investigate mass transfer and phase-structure transformations in the surface layer. The probable mechanisms of layer formation are discussed, which comprise electrochemical oxidation of the Ti-electrode by OH⁻ anions, complimented by chemical precipitation of Al(OH)₃ and plasma-induced transformations in the surface discharges. Running with a total yield efficiency of 20–30%, these processes lead to the formation of predominantly the Al₂TiO₅ phase with heterogeneous precipitation of Al₂TiO₅·TiO₂ and 3Al₂TiO₅·Al₂O₃ eutectics. Al- and Ti-enriched constituents of this structure show hardnesses of 1050–1480 and 300–845 H_K, 0.02, respectively. The layer growth rate increases with increasing electrolyte concentration, providing a maximum thickness of over 60 μm and a surface roughness (R_a) of 3–4 μm. Increasing the electrolyte pH from 12.0 to 12.8 results in smoothing and thickening of the surface layer but a lower sample weight gain, associated with an enhancement of the Ti electro-oxidation process. Morphological changes during PEO formation of the surface layer include gradual transformation of the original fine grained but porous structure into a dense, fused morphology which is adversely affected by discharge-induced thermal stresses, causing a degradation of the layer adhesion strength.     

Crystal growth of superconductive PrBa2Cu3O7−y

Superconductive PrBa₂Cu₃O_7−y (Pr123) crystals have been grown successfully by the travelling-solvent floating-zone (TSFZ) method using 3.7–5.8% PrO, 27–37% BaO, and 60–69% CuO composition solution with the 0.1–0.4% oxygen mixed argon gas atmosphere. The grown crystals have been identified to be Pr123 by a precession camera, X-ray powder diffractions and scanning electron microscopy–X-ray energy dispersion spectroscopy (SEM-EDS). Some portion of the grown TSFZ crystal boules show bulk superconductivity below about 80 K after annealing in oxygen.     

Magnetic properties of Sm–Co–B-based nanocomposite magnets

The magnetic properties of nanocomposite melt-spun magnets with composition Sm_16−xCo_68+xB₁₆ (x=0–10, 2 at% interval) and Sm₈Co_92−yB_y (y=10–18, 2 at% interval) have been studied systematically. Several ribbons were fabricated with a wheel speed of 50 m/s, followed by annealing in the temperature range of 700–800°C for 2.5–40 min. XRD results and magnetization versus temperature curves showed that almost all of the samples were composed of the tetragonal Sm₂Co₁₄B and rhombohedral SmCo₁₂B₆ phases which are not magnetically hard at room temperature. However, a relatively high coercivity in the range of 3.5–5.5 kOe has been obtained in these samples. The highest coercivity of 5.5 kOe and a very promising β value of −0.28%/°C were obtained in Sm₈Co₇₄B₁₈ ribbons annealed at 750°C for 5 min. The high coercivities are attributed to the small grain size of the 2 : 14 : 1 phase, in which the large surface areas enhance its effective anisotropy, and make it uniaxial type.     

Study of effects of Mn in CdS nanocrystals

Mn²⁺-doped CdS nanocrystals have been synthesized by adopting an aqueous solution precipitation method. These nanocrystals have been studied using X-ray diffraction (XRD), X-ray fluorescence (XRF), optical absorbance, photoluminescence (PL), DC electrical conductivity measurements and positron annihilation lifetime spectroscopy (PALS). The system has been found to be in the hexagonal phase. PL spectra have been studied on most prominent exciton peaks within the wavelength range (586–731 nm). The emission intensity is found to increase on increasing Mn²⁺ ion concentration (0–5%). Electrical conductivity lies within 0.819×10⁻⁶ to 1.69×10⁻⁶ Ω⁻¹ m⁻¹ and the system shows power law dependence for n=3–3.77. The Cd vacancies concentration has been found to decrease on increasing Mn%.     

Laser ablated bismuth cuprate thin films preparation and effect of oxygen nonstoichiometry upon superconductivity

Thin films of Bi₂Sr₂CaCu₂O₈ and (Bi, Pb)₂Sr₂Ca₂Cu₃O₁₀ have been prepared on monocrystalline (100) MgO substrates, using a laser ablation method with post annealing treatment. The influence of substrate temperature and oxygen pressure during deposition were investigated. SEM observations, EDS analysis, electric and magnetic measurements have been used to characterize the films. Superconducting “2212” films, with T_c(R = 0) at 80–83 K and J_c (50 K) up to 5 × 10⁵ A/cm², have been currently achieved, while Pb-doped “2223” films exhibit T_c as high as 110 K with J_c = 5 × 10⁴ A/cm² at 77 K. The effect of annealing at low temperature (350°C) in an argon flow has been studied for the 2212 phase, it shows the influence of the oxygen non-stoichiometry, i.e. of the hole carrier density upon T_c's which can be measured up to 89 K (zero resistance).     

Anelastic relaxation of Pr1/2Ca1/2MnO3 at low and medium frequencies in the 350–500 K range

In previous works (Jornadas SAM 2000; J. Magn. Magn. Mater. 226–230 (2001) 988) the low-frequency anelastic effects of two manganite perovskites of La_2/3Sr_1/3MnO₃ and La_2/3Ca_1/3MnO₃ were studied at 1 Hz and temperatures above those of the metal–insulator transition. An important internal friction peak (P1) appears at 414 and 419 K, respectively, with a modulus variation and no appreciable contribution to electrical resistivity. Another compound Pr_1/2Ca_1/2MnO₃ of the same family has been studied by anelastic mechanical spectroscopy in order to add new data which could elucidate the (P1) peak mechanism. The measurements were made in a sub-resonant forced pendulum (0.1–20 Hz) and in a vibrating reed equipment (kHz range). A stable (P1) peak has been detected at 410 K (1 Hz), with a corresponding modulus step. The appearance of this relaxation peak in the Pr_1/2Ca_1/2MnO₃ compound, and its high activation energy value, similar to the other compounds measured, indicates that the microscopic origin of this relaxation does not correspond to an oxygen jump (characteristic activation energy0.8–0.9 eV).     

Investigations of heavy ion tracks in polyethylene naphthalate films

The heavy ion beam (with fluence 3x10⁸ ion/cm²) from a cyclotron has been used for irradiation of thin polyethylene naphthalate (PEN) films. Latent tracks in these polymeric films have been sensitized by UV radiation and then chemically etched in NaOH solution. The etching process parameters have been controlled by the electroconductivity method. After etching, parameters of samples have been examined by SEM and bubble point methods (Coulter® Porometer II instrument). Results have shown good quality of PEN track membranes with pore sizes in the range: 0.1 – 0.5 μm. The described procedure is known for thin polythylene terephthalate (PET) films. Taking into consideration that PEN films have got better mechanical, thermal, gas barrier as well as better chemical resistance properties in comparison with PET films, the possibility of application of such membranes is much wider.     

Structural evolution of Sc-containing zirconia electrolytes

A powder of nominal composition (ZrO₂)_0.886(Sc₂O₃)_0.104(Al₂O₃)_0.01 was synthesized by spray drying with the purpose of testing the performance of solid oxide fuel cells containing scandia-stabilized zirconia (ScSZ) as electrolyte. The phases resulting from calcination and sintering at different temperatures were investigated by XRD, impedance and Raman spectroscopy. At sintering temperatures of 1200–1400 °C nearly equal amounts of cubic and rhombohedral ScSZ were detected, whereas heat treatment higher than 1500 °C led to a cubic single-phase material. A preliminary reaction mechanism of phase formation is proposed with respect to the various results depending on heat treatment.     

Viscoelastic investigation by ultrasonic shear waves of liquid eutectic mixture methylurea–ammonium sulfamate

Shear impedance of the liquid eutectic mixture CH₃NHCONH₂–NH₄SO₃NH₂ was studied in the temperature range 291.7–313.2 K by using ultrasonic shear waves in the frequency range 12–80 MHz. Ultrasonic technique allowed the determination of the real part of the complex mechanical impedance and of the complex rigidity modulus. The relaxation region was shifted towards higher frequency in comparison to the Maxwell model and was fitted by the modified BEL model.     

Monte Carlo study of the magnetic properties of Fe0.9−qMn0.1Alq-disordered alloys

Within the framework of a random site-diluted Ising model with nearest-neighbor interactions, and using the Metropolis algorithm for equilibration and energy minimization, we have computed the ensemble and configurational averages for magnetization per site, magnetic susceptibility and specific heat of Fe_0.9−qMn_0.1Al_q-disordered alloys with 0.1q0.55. In the model, atoms have been randomly distributed on a body-centered cubic lattice in order to simulate the disorder and structure as that obtained in arc-melted Fe_0.9−qMn_0.1Al_q alloys treated at high temperatures during long periods of time and followed by fast quenching. Competitive interactions coming from Fe–Fe ferromagnetic bonds and Fe–Mn and Mn–Mn antiferromagnetic couplings, as well as the Al dilutor effect, have been taken into account in our study. Results allow us to conclude that, in agreement with previous Mössbauer data of the average hyperfine field, for which a comparison is also carried out, the Fe_0.9−qMn_0.1Al_q-disordered alloys are well characterized by a critical concentration at room temperature at around 40 at% Al, for which the system undergoes a transition from a ferromagnetic state to a paramagnetic one. The finite size scaling analysis to obtain the critical Al concentration in the thermodynamic limit, as well as the critical exponents, is also presented and discussed.