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.     

Absorbed dose evaluations in retrospective dosimetry: methodological developments using quartz

Dose evaluation procedures based on luminescence techniques were applied to 50 quartz samples extracted from bricks that had been obtained from populated or partly populated settlements in Russia and Ukraine downwind of the Chernobyl NPP. Determinations of accrued dose in the range 30–300 mGy were obtained using TL (210°C TL and pre-dose) and OSL (single and multiple aliquot) procedures. Overall, good inter-laboratory concordance of dose evaluations was achieved, with a variance (1σ) of ±10 mGy for the samples examined.     

Characteristics of TL and PTTL glow curves of gamma irradiated pure Li2B4O7 single crystals

The TL glow curve of X-ray irradiated pure and Cu-doped Li₂B₄O₇ shows that the most intense TL peak is at 160°C. In the present work the characteristics of the TL and PTTL glow curves from gamma irradiated pure Li₂B₄O₇ single crystal samples (prepared by Mitui Kinzoku Kougyo, Japan) have been studied. The samples were irradiated with different gamma doses (from 0.5 up to 500 Gy) using a ⁶⁰Co gamma ray source at a dose rate of 78 Gy h⁻¹. The TL glow curve shows three intense peaks (at 160°C, 260 and 305°C) and three weak ones (at 110, 140 and 220°C). The most intense TL peak is at 160°C, which agrees with the TL glow curve from X-ray irradiated samples [Kutomi Y. and Tomita A. (1990) TSEE and TL of Li₂B₄O₇:Cu single crystals. Radiat. Prot. Dosim. 33, 347–350]. The 305°C peak in gamma irradiated samples also appears to be very intense, which indicates its possible use in high-dose high-temperature dosimetry. Further, the characteristics of the PTTL glow curve have been studied as a function of ultraviolet exposure and number of repeated PTTL cycles.     

TL and PTTL in natural fluorite previously irradiated with gamma rays and heavy ions

The effect of annealing temperature on the phototransfer thermoluminescence (PTTL) signal was studied to determine the appropriate annealing temperature for treating the natural powder before irradiation. The temperatures used to anneal virgin natural fluorite samples (only natural dose without giving the samples any artificial doses) were 150, 250, 350, 450, 550, 650 and 750°C for a duration of 1 h in each case. The results show that the PTTL response did not change for anneal temperatures up to 450°C, but at higher temperatures the signal decreased rapidly. The height of the 90°C peak decreased by two orders of magnitude as the anneal temperature increased from 450 to 750°C, whilst the height of the 180°C peak decreased by three orders of magnitude between the same two annealing temperatures. In order to investigate the effect of previous gamma rays and heavy ion irradiation on thermoluminescence (TL) and PTTL signals, powdered samples of natural fluorite from Cornwall, England, were annealed at 500°C and then irradiated (at GSI, Darmstadt, Germany) with ¹⁶¹Dy ions of energy 13 Mev/n; the range of fluences used was from 10⁴ to 10¹² ion cm⁻². Identical samples were given gamma doses in the range 1 Gy to 2.6 × 10⁴ Gy in order to compare the effects of gamma rays and heavy ions. The sensitivities of TL and PTTL were studied by giving the samples a gamma test dose of 1 Gy after annealing the samples at 500°C for 30 min in order to eliminate the TL resulting from previous gamma or heavy ion irradiation.     

Synthesis and physical behaviour of In2S3 films

In₂S₃ layers have been grown by close-spaced evaporation of pre-synthesized In₂S₃ powder from its constituent elements. The layers were deposited on glass substrates at temperatures in the range, 200–350 °C. The effect of substrate temperature on composition, structure, morphology, electrical and optical properties of the as-grown indium sulfide films has been studied. The synthesized powder exhibited cubic structure with a grain size of 63.92 nm and S/In ratio of 1.01. The films grown at 200 °C were amorphous in nature while its crystallinity increased with the increase of substrate temperature to 300 °C. The films exhibited pure tetragonal β-In₂S₃ phase at the substrate temperature of 350 °C. The surface morphological analysis revealed that the films grown at 300 °C had an average roughness of 1.43 nm. These films showed a S/In ratio of 0.98 and a lower electrical resistivity of 1.28 × 10³ Ω cm. The optical band gap was found to be direct and the layers grown at 300 °C showed a higher optical transmittance of 78% and an energy band gap of 2.49 eV.     

RF-sputtered CrB2 diffusion barrier for Ni/Au Ohmic contacts on p-CuCrO2

Ohmic contacts to p-type CuCrO₂ using Ni/Au/CrB₂/Ti/Au contact metallurgy are reported. The samples were annealed in the 200–700 °C range for 60 s in flowing oxygen ambient. A minimum specific contact resistance of 2 × 10⁻⁵ Ω cm² was obtained after annealing at 400 °C. Further increase in the annealing temperature (>400 °C) resulted in the degradation of contact resistance. Auger Electron Spectroscopy (AES) depth profiling showed that out-diffusion of Ti to the surface of the contact stacks was evident by 400 °C, followed by Cr at higher temperature. The CrB₂ diffusion barrier decreases the specific contact resistance by almost two orders of magnitude relative to Ni/Au alone.     

Defect versus nanocrystal luminescence emitted from room temperature and hot-implanted SiO2 layers

Silicon nanocrystals have been synthesized in SiO₂ matrix using Si ion implantation. Si ions were implanted into 300-nm-thick SiO₂ films grown on crystalline Si at energies of 30–55 keV, and with doses of 5×10¹⁵, 3×10¹⁶, and 1×10¹⁷ cm⁻². Implanted samples were subsequently annealed in an N₂ ambient at 500–1100°C during various periods. Photoluminescence spectra for the sample implanted with 1×10¹⁷ cm⁻² at 55 keV show that red luminescence (750 nm) related to Si-nanocrystals clearly increases with annealing temperature and time in intensity, and that weak orange luminescence (600 nm) is observed after annealing at low temperatures of 500°C and 800°C. The luminescence around 600 nm becomes very intense when a thin SiO₂ sample is implanted at a substrate temperature of 400°C with an energy of 30 keV and a low dose of 5×10¹⁵ cm⁻². It vanishes after annealing at 800°C for 30 min. We conclude that this luminescence observed around 600 nm is caused by some radiative defects formed in Si-implanted SiO₂.     

Superconducting Nd1.85Ce0.15CuO4 films grown by the pulsed electron deposition technique

Nd_1.85Ce_0.15CuO_4−δ superconducting thin films were prepared on (1 0 0) SrTiO₃ substrates by pulsed electron deposition technique without reducing atmosphere. Oxygen content is finely controlled by high temperature vacuum annealing, and optimal superconductivity has been obtained. The deposition conditions of the film are discussed in details. Higher deposition temperature and lower gas pressure result in the loss of copper and the appearance of the foreign phase Ce_0.5Nd_0.5O_1.75. High quality Nd_1.85Ce_0.15CuO_4−δ epitaxial films are deposited at 840–870 °C in the mixed gas with a ratio of O₂:Ar = 1:3.     

OSL from BeO ceramics: new observations from an old material

In BeO ceramics, exposed to ionizing radiation, an intense OSL signal was observed. The properties of the signal and its behavior under various experimental conditions were investigated. It was found that the OSL signal is a composite signal and exhibits strong thermal quenching. The quenching energy was estimated as 0.5 eV. The excitation spectrum of the OSL signal was obtained as a broad peak in the region 420–550 nm with maximum around 435 nm. The possible correlation between the OSL signal and the peaks in the TL glow curve was also examined. It was interesting to observe that the highly light sensitive TL peak near 220°C does not contribute to the OSL signal. The OSL signal was found to originate from a trap near 340°C.

To check the possibility of using the material for radiation dosimetry the dose response and thermal stability of the OSL signal were also investigated. The dose response was found to be quite linear up to 10 Gy. The thermal activation energy of the OSL trap was determined as 1.7 eV using isothermal annealing and heating rate methods thus proving the suitability for dosimetry.     

Phase evolution during the melting and recrystallization of ceramic core in the (Bi,Pb)-2223 tape

The phase evolution during melting and recrystallization of (Bi,Pb)₂Sr₂Ca₂Cu₃O₁₀ ((Bi,Pb)-2223) core in a Ag-sheathed monofilamentary tape has been investigated. The tape was fabricated by PIT process with powders containing nearly pure (Bi,Pb)-2223 phase. Short samples were melted at 805 °C, 808 °C, 812 °C, 816 °C, 831 °C, slowly cooled at 1.5 °C/h under flowing 1.6% O₂ balanced with argon and quenched in air at room temperature. X-ray diffraction (XRD) and scanning electron microscopy coupled with energy dispersive spectroscopy (SEM/EDS) were applied for the phase identification. The results show that (Bi,Pb)-2223 core is partially melted into a liquid and alkaline earth cuprates (AECs), mainly 2:1-AEC, at 805 °C, 808 °C, 812 °C, and well reforms directly from the melt during the slow cooling. More (Bi,Pb)-2223 phase is decomposed at temperatures higher than 816 °C, but cannot recrystallize, indicating that a partial melting at some temperatures around a given temperature range is essential to (Bi,Pb)-2223 phase reformation. The melt composition moves from that between “2223” and “2212” stoichiometries towards 2212-like stoichiometry with increasing temperature. This seems to lead to the conclusion that (Bi,Pb)-2223 phase decomposes incongruently into a 2212-like liquid and (Ca,Sr)-cuprates. 2:1-AEC plays the most important role in (Bi,Pb)-2223 melt-recrystallization process. Our results also reveal that plate-like shape (Bi,Pb)-2223 grains can be obtained via melting and recrystallization if the optimum processing conditions are used.     

The use of polarization modulation and amplitude-sensitive optical heterodyne interferometry for linear birefringence parameters measurement

A novel common-path polarization modulation and amplitude-sensitive optical heterodyne polarimeter is setup in order to characterize a phase retardation plate (PRP) in real time. The phase retardation ΔΦ and fast-axis angle β of the linear birefringence parameters (LBP) of a PRP are measured simultaneously. Meanwhile, the dynamic ranges of 0° < ΔΦ < 180° and 0° < β < 180° are demonstrated experimentally. In order to measure LBP in real time, a polarization modulation is introduced by continuously rotating the tested PRP such that ΔΦ and β are able to be obtained in terms of the ratio of the amplitudes of S polarization and the ratio of P polarization of the heterodyne signals, respectively. Consequently, this novel method, which combines optical heterodyne interferometry with a polarization modulation technique, not only improves the detection sensitivity, but also provides a real time capability to measure LBP. In addition, the error in the LBP measurement is derived and analyzed.     

Fabrication of p-Si/β-FeSi2 balls/n-si structures by MBE and their electrical and optical properties

We report on the formation technique of single-crystalline β-FeSi₂ balls (<100 nm) embedded in a Si p–n junction region by Si molecular beam epitaxy (MBE). β-FeSi₂ films grown on Si (0 0 1) by reactive deposition epitaxy (RDE) aggregated into islands after annealing at 850°C in ultrahigh vacuum. The islands of β-FeSi₂ aggregated further into a ball shape by following the Si MBE overgrowth at 750°C. It was found from X-ray diffraction (XRD) patterns that the epitaxial relationship between the two materials, and single-crystalline nature were preserved even after the annealing and the Si overgrowth. Capacitance–voltage (C–V) characteristics and transmission electron microscope (TEM) images revealed that a lot of defects were introduced around the embedded β-FeSi₂ balls with an increase of embedded β-FeSi₂ quantity.     

Ln1−xSrxCoO3(Ln = Sm, Dy) for the electrode of solid oxide fuel cells

The perovskite-type oxides were synthesized in the series of Ln_1−xSr_xCoO₃(Ln = Sm, Dy). The formation of solid solutions in Dy_{1 − x}Sr_xCoO₃ was limited, compared with that in Sm_{1 − x}Sr_xCoO₃. The electrical conductivities of the sintered samples were measured as a function of x in the temperature range 30 to 1000 °C. The highest conductivity of around 500 S/cm at 1000 °C was found in Sm_0.7Sr_0.3CoO₃. The reactivity of all the samples with YSZ was examined at 800–1000 °C for 96 h. The Sr-doped perovskite oxides were more reactive with YSZ and produced SrZrO₃ at 900 °C after 96 h. However, no reaction product between SmCoO₃ and YSZ was observed at 1000 °C for 96 h. The cathodic polarization of the oxide electrodes, sputtered on yttria stabilized zirconia (YSZ), was studied at 800–1000 °C in air. SmCoO₃ shows no degradation of the electrode performance at higher temperatures. The thermal expansion measurements on the sintered samples were carried out from room temperature to 1000 °C. Large thermal expansion coefficients were found in these samples.     

Enhanced magnetic properties of Nd–Fe–B thin films crystallized by heat treatment

Nd₂Fe₁₄B Φ phase crystallites were formed in Nd_16.7Fe_65.5B_17.8 thin films prepared by RF sputtering with subsequent heat treatment. The 2 μm-thick films were deposited onto 0.1 mm Mo sheets at an average substrate temperature (T_s) of 365°C. The enhanced magnetic properties of the magnetically anisotropic thin films were investigated using different heating rates (h_r) of 10°C, 20°C, 50°C and 100°C/min in an annealing experiment. Transformation from the amorphous phase to the crystalline phase is clearly manifested by the formation of fine crystallites embedded as a columnar matrix of Nd₂Fe₁₄B phase. High-resolution scanning electron microscope data of the cross-section of the annealed films show columnar stacking of Nd₂Fe₁₄B crystallites with sizes <500 nm. Transmission electron microscope observations revealed that the microstructure of these films having out-of-plane magnetization consists of uniformly distributed Φ phase with grain size around 400 nm together with small Nd rich particles. This grain size of Φ phase is comparable to the single domain particle diameter of Nd₂Fe₁₄B. Significant change in _iH_c, 4πM_r and 4πM_s with h_r was confirmed. Annealing conditions with a heating rate of 50°C/min to an annealing temperature (T_a) of 650°C for 30 min was consequently found to give optimum properties for the NdFeB thin films. The resulting magnetic properties, considered to be the effect of varying h_r were _iH_c= 1307–1357 kA/m, 4πM_r=0.78–1.06 T and 4πM_s=0.81–1.07 T.     

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.     

Luminescence from γ-irradiated humic acid

This study was conducted to investigate the ultraweak delayed radiochemiluminescence (RCL) spectra, kinetics and spectroscopic properties of humic acids (HAs) after γ-radiation exposure (absorbed doses of 1−10 kGy, Co-60) in model systems.

The kinetics and spectral distribution of RCL (340–650 nm) were measured using the single photon counting (SPC) method and cut-off filters.

The intensity of fluorescence (λ_ex=390, 440, 490 and 540 nm) covering the spectral range 400–580 nm was heavily dependent on the λ_ex and slightly increased with the absorbed dose of γ-radiation.

Absorption spectra (the range 240−800 nm) and color coefficients E_2.6/4 and E_4/6 of irradiated solutions indicated that post-radiative degradation/polymerization processes take place in the HA, changing their macromolecule size or properties.

Comparison of FTIR spectra and elemental analysis proved an increased O and decreased C atoms in irradiated samples. The data indicate on the radiolysis-induced degradation of native HA into fulvic-like acids with higher hydrophilicity and lower molecular size.     

Radioluminescence (RL) behaviour of Al2O3:C-potential for dosimetric applications

The radioluminescence (RL) of carbon doped aluminium oxide (Al₂O₃:C) TL dosimeter material (TLD-500) was investigated using a ¹³⁷Cs conversion electron source (which also emits β and γ) for simultaneous irradiation and luminescence excitation. Furthermore, RL dosimetry characteristics of this material were studied. The main RL emission occurs at 420 nm. That matches the known main TL and OSL emissions for this material as well as an emission that was investigated in earlier RL studies, excited at higher energies (4 MeV electrons) and very high pulse delivered doses (≈800 kGy·s⁻¹). Furthermore, the saturation dose for the main peak is reached at the dose level of ≈80 Gy as known from TL and earlier RL investigations. Other peaks at 700 and 790 nm and broad emission bands at photon energies higher than 3.00 eV and others between 2.00 and 2.50 eV were observed. The 700 nm emission shows growth also at higher dose levels, and saturates at an estimated dose of ≈800 Gy. The 790 nm emission reaches its maximum intensity at ≈10 Gy absorbed dose. The reported results give an outlook to the usability and the potential of Al₂O₃:C combined with RL measurements for radiation dosimetry as well as for beta source calibration, using radioluminescence.     

Effect of Cu doping in MgB2 superconductor at various processing temperatures

The effects of Cu doping in MgB₂ superconductor has been studied at different processing temperatures. The polycrystalline samples of Mg_1−xCu_xB₂ with x = 0.05 were synthesized through the in-situ solid sate reaction method in argon atmosphere at different temperature range between 800–900 °C. The samples were characterized through X-ray diffraction (XRD), Scanning Electron Microscopy (SEM) and low temperature R–T measurement techniques for the phase verification, microstructure and superconducting transition temperature, respectively. The XRD patterns of Mg_1−xCu_xB₂ (x = 0.05) do not exhibit any impurity traces of MgB₄ or MgB₆ and they show the sharp transition in the samples prepared at 850 °C. The onset transition temperature of the prepared samples is around 39 K, which is almost the same as that for the pure MgB₂. This indicates that Cu doping in MgB₂ does not affect the transition temperature. The SEM micrograph of Mg_0.95Cu_0.05B₂ has shown that the sample is dense with grain size smaller than 1 μm.     

The IR spectra of Mg5C(CO) complexes on the (0 0 1) surfaces of polycrystalline and single crystal MgO

The FTIR spectroscopy of carbon monoxide adsorbed on polycrystalline MgO smoke has been investigated as a function of the CO equilibrium pressure at constant temperature (60 K) (optical isotherm) and of the temperature (in the 300–60 K range) at constant CO pressure (optical isobar). In both cases the spectra fully reproduce those of CO adsorbed on the (0 0 1) surface of UHV cleaved single crystals [Heidberg et al., Surf. Sci. 331–333 (1995) 1467]. This result, never attained in previous investigations on dispersed MgO, contribute to bridging the gap which is commonly supposed to exist between surface science and the study of “real” (defective) systems. Depending on the surface coverage θ the main spectral features due to the CO/MgO smoke interaction are a single band shifting from 2157.5 (at θ→0) to 2150.2 cm⁻¹ (at θ=1/4) or a triplet, at 2151.5, 2137.2 and 2132.4 cm⁻¹ (at θ>1/4). These manifestations are due to the ν(CO) modes of Mg_5C²⁺· · · CO adducts formed on the (0 0 1) terminations of the cubic MgO smoke microcrystals. The formation of the CO monolayer is occurring in two different phases: (i) a first phase with CO oscillators perpendicularly oriented to the surface (2157–2150 cm⁻¹) and (ii) a second phase constituted by an array of coexisting perpendicular and tilted species (triplet at 2151.5, 2137.2 and 2132.4 cm⁻¹). A much weaker feature at 2167.5–2164 cm⁻¹ is assigned to Mg_4C²⁺· · · CO adducts at the edges of the microcrystals. The heat of adsorption of the perpendicular Mg_5C²⁺· · · CO complex in the first phase has been estimated from the optical isobar and results to be 11 kJ mol⁻¹.     

Optically stimulated luminescence (OSL) study of synthetic stishovite

Optically stimulated luminescence (OSL) of synthetic stishovite was investigated for a future dating technique of meteor impact craters. Luminescence around 330 nm was measured on the γ-ray irradiated stishovite under two stimulating light sources of infrared laser (830 nm) and blue light emitting diode set (470 nm). Thermoluminescence (TL) studies before and after the OSL measurements showed the intensities around 100–200°C and 220–350°C to increase and those around 350–450°C to decrease. This indicates that a part of deep-trapped charges excited during the OSL measurements were retrapped by shallower traps. The infrared stimulated luminescence (IRSL) after the TL measurement up to 450°C could not be detected, while the blue light stimulated luminescence (BLSL) after TL had about one-tenth of the intensity before TL. This indicates that a part of the charges in shallower traps were detrapped thermally and returned to the deeper traps which were related to BLSL. The result implies that some of the BLSL-related traps are quite stable at room temperature and could be used for geological dating. In addition, two paramagnetic centers produced by sudden release of high pressure in synthesis process were found in the unirradiated stishovite by electron spin resonance (ESR). Their g-factors are g=2.00181 and g=2.00062 for an axial signal and g=2.00305 for the other isotropic signal. These signals could be used for an evidence of impacts if those signals could be stored in geological time.