Laser and plasma nitriding of titanium using CW-CO2 laser in the atmosphere

Surface nitriding of the titanium by the mixing technology with laser and plasma (LPN) in atmosphere has been investigated. Comparing with the technique of laser nitriding, we could obtain the titanium nitride at relatively low laser power density and the oxidation was prevented without the chamber. The synthesized layers comprised of titanium nitrides were about 178 μm depth. The effect of the laser power density, scanning velocity, and plasma flow rate on the components consisting of the material of the nitrided layer was studied. X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS) were used to reveal the components consisting of the material of the nitrided layer.     

Synthesis of carbon nanotubes via Fe-catalyzed pyrolysis of phenolic resin

Carbon nanotubes (CNTs) with 40–100 nm in diameter and tens of micrometers in length were prepared via catalytic pyrolysis of phenol resin in Ar at 673–1273 K using ferric nitrate as a catalyst precursor. Structure and morphology of pyrolyzed resin were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and Raman spectroscopy. Ferric nitrate was transformed to Fe₃O₄ at 673 K, and to metallic Fe and Fe_xC carbide at 873–1273 K. The optimal weight ratio of Fe catalyst to phenol resin for growing CNTs was 1.00 wt%, and the optimal temperature was 1073 K. In addition, use of a high pressure increased the yield of CNTs. Density functional theory (DFT) calculations suggest that Fe catalysts facilitate the CNTs growth by increasing the bond length and weakening the bond strength in C₂H₄ via donating electrons to the C atoms in it.     

Charge transport in polycrystalline titanium dioxide☆

This work reports semiconducting properties of undoped polycrystalline TiO₂ studied using the measurements of the electrical conductivity (EC) and thermopower as a function of oxygen partial pressure and temperature in the ranges of p(O₂) between 10 Pa and 70 kPa and temperature 1173–1273 K. The width of the band gap, determined from the minimum of EC, is equal to 3.055±0.012 eV. It was found that the apparent concentration of negatively charged defects, involving both acceptor-type aliovalent ions and Ti vacancies, increases with temperature from 0.6 at% at 1173 K to the level of 0.9–1.4 at% at 1273 K. This effect is considered in terms of Schottky-type defects. It was observed that the minimum of EC at the n–p transition is lower than that for TiO₂ single crystal thus suggesting that grain boundaries are responsible for the formation of conductivity weak links.     

Photoelectrochemical characterization of annealed cadmium selenide photoelectrode using sulphide–polysulphide electrolyte

Cadmium selenide films have been synthesized by dip method. Cadmium selenide acts as photoanode in photoelectrochemical (PEC) cells. The photoanode was annealed upto 473 K. The cell configuration is n-CdSe∣NaOH (1 M) +S (1 M) +Na₂S (1 M) ∣C_(graphite). Various performance parameters were examined with respect to annealed temperature. It is found that the fill factor and efficiency are maximum for photoelectrode annealed at 473 K. This is due to low resistance, high flat-band potential, maximum open-circuit voltage as well as maximum short-circuit current. The barrier height was examined from the temperature dependence of the reverse saturation current. The lighted ideality factor was found to be minimum for photoelectrode annealed at 473 K. A cell utilizing annealed photoelectrode showed a wider spectral response. The utility of this work is in improving the efficiency of PEC cells.     

Fabrication of Gd0.5Sr0.5CoO3 film for SOFC cathode by pulsed laser deposition

Gd_0.5Sr_0.5CoO₃ (GSCO) film has been fabricated by pulsed laser deposition (PLD) to be used as the cathode of the solid oxide fuel cell (SOFC). The GSCO thin film obtained has a columnar crystalline structure so that it will have a high permeation property. The PLD technique has been found suitable for growing a film of complex composition because of its good control of stoichiometry and thus for fabricating a GSCO film used as the cathode of the SOFC. The GSCO film has been studied for porosity electrical conductivity and power density. The GSCO film grown at a substrate temperature of 1100 K and oxygen gas pressure of 100 Pa has high electrical conductivity which is 820 S cm^− 1 at 973 K with post annealing at a rather low temperature (1000 K). This value is higher than that of the GSCO film prepared by RF-sputtering with post annealing at a higher temperature (1273 K).     

Application of indium tin oxide (ITO) thin film as a low emissivity film on Ni-based alloy at high temperature

Indium tin oxide (ITO) films as the low emissivity coatings of Ni-based alloy at high temperature were studies. ITO films were deposited on the polished surface of alloy K424 by direct current magnetron sputtering. These ITO-coated samples were heat-treated in air at 600–900 °C for 150 h to explore the effect of high temperature environment on the emissivity. The samples were analyzed by X-ray diffraction (XRD), SEM and EDS. The results show that the surface of sample is integrity after heat processing at 700 °C and below it. A small amount of fine crack is observed on the surface of sample heated at 800 °C and Ti oxide appears. There are lots of fine cracks on the sample annealed at 900 °C and a large number of various oxides are detected. The average infrared emissivities at 3–5 μm and 8–14 μm wavebands were tested by an infrared emissivity measurement instrument. The results show the emissivity of the sample after annealed at 600 and 700 °C is still kept at a low value as the sample before annealed. The ITO film can be used as a low emissivity coating of super alloy K424 up to 700 °C.     

Conductivity and dielectric relaxation phenomena in (NH4)2SO4 single crystal

AC impedance measurements have been carried out on (NH₄)₂SO₄ single crystals for the temperatures from 300 to 473 K and frequency range between 100 Hz and 4 MHz. The results reveal two distinct relaxation processes in the sample crystal. One is the dipolar relaxation with a peak at frequency slightly higher than 4 × 10⁶ Hz. The other is the charge carrier relaxation at lower frequencies. The frequency dependence of conductivity is described by the relation σ(ω) = Bωⁿ, and n = 1.32 is obtained at temperatures below 413 K. This value drops to 0.2 and then decreases slightly with increasing temperature. The dipolar response of the (NH₄)₂SO₄ single crystal under an ac field is attributed to the reorientation of dipoles. The contribution of charge carriers is increasing substantially with increasing temperature at temperatures above 413 K. The temperature variation of conductivity relaxation peaks follows the Arrhenius relation. The obtained activation energy for migration of the mobile ions for (NH₄)₂SO₄ single crystal was 1.24 eV in the temperature range between 433 and 468 K in this intrinsic region. It is proposed that the NH₄⁺ in the sample crystal has the contribution to the electrical conduction.     

Effects of Zr impurity on microscopic behavior of Hf metal

Hf metal with ∼ 3 wt% Zr impurity has been reinvestigated by perturbed angular correlation (PAC) spectroscopy using a LaBr₃(Ce)–BaF₂ detector set up to understand the microscopic behavior of this metal with temperature. From present measurements, five quadrupole interaction frequencies have been found at room temperature where both pure hcp fraction (∼33%) with 12 nearest neighbor Hf surrounding the probe ¹⁸¹Hf atom and the probe–impurity fraction (∼33%) corresponding to 11 nearest neighbor Hf plus one dissimilar Zr atom are clearly distinguished. At room temperature, the results for quadrupole frequency and asymmetry parameter are found to be ω_Q=51.6(4) Mrad/s, η=0.20(4) for the impurity fraction and ω_Q=46.8(2) Mrad/s, η=0 for the pure fraction with values of frequency distribution width δ=0 for both components. At 77 K, only 1 NN Zr impurity (∼93%) and pure hcp (∼7%) components have been found with a value of δ ∼ 10% for the impurity fraction. A drastic change in microstructural configuration of Hf metal is observed at 473 K where the impurity fraction increases to ∼ 50% and the pure hcp fraction reduces to ∼ 15% with abrupt changes in quadrupole frequencies for both components. The pure fraction then increases with temperature and enhances to ∼50% at 973 K. In the temperature range 473–973 K, quadrupole frequencies for both components are found to decrease slowly with temperature. Using the Arrhenius relation, binding energy (B) for the probe–impurity pair and the entropy of formation are measured from temperature dependent fractions of probe–impurity and pure hcp in the temperature range 473–773 K. The three other minor components found at different temperatures are attributed to crystalline defects.     

Mid-infrared photoconductive properties of heavily Bi-doped PbTe p–n homojunction diode grown by liquid-phase epitaxy

We fabricated a heavily Bi-doped (x_Bi ≈ 2 × 10¹⁹ cm⁻³) PbTe p–n homojunction diode that detects mid-infrared wavelengths by the temperature difference method (TDM) under controlled vapor pressure (CVP) liquid phase epitaxy (LPE). The photocurrent density produced by the heavily Bi-doped diode sample is approximately 20 times and 3 times greater than that produced by an undoped and heavily In-doped sample, respectively. By varying the ambient temperature from 15 K to 225 K, the detectable wavelength is tunable from 6.18 μm to 4.20 μm. The peak shift of the detectable wavelength is shorter in the heavily Bi-doped sample than in the undoped sample, consistent with our previously proposed model, in which Bi–Bi nearest donor–acceptor pairs are formed in the heavily Bi-doped PbTe liquid phase epitaxial layer. Current–voltage (I–V) measurements of the heavily Bi-doped diode sample under infrared exposure at 77 K indicated a likely leak in the dark current, arising from the deeper levels. From the dark I–V measurements, the activation energy of the deep level was estimated as 0.067 eV, close to the energy of the deep Tl-doped PbTe acceptor layer. We conclude that the deep level originates from the Tl-doped p-type epitaxial layer.     

XRD and Mössbauer spectroscopy investigation of Fe2O3–Al2O3 nano-composite

Fe₂O₃–Al₂O₃ nano-composites were synthesized by sol–gel means. The properties of samples sintered at various thermal treatment temperatures were investigated by X-ray diffraction (XRD) and Mössbauer spectroscopy (MS). The experimental results show that the γ- to α-Al₂O₃ transformation occurs at lower temperature after iron oxide doping. The samples obtained at 1173 K contained poorly crystallized γ-Al₂O₃ phase and an amorphous iron oxide. When the temperature of heating was increased to 1373 K, the sample was composed of α-Fe₂O₃/α-Al₂O₃ nano-composite and some solid solution. A superparamagnetic phenomenon was observed until the thermal treatment temperature reached 1373 K.     

Surface engineering of biomedical metallic materials by plasma-based low-energy ion implantation

Plasma-based low-energy ion implantation, including plasma source ion nitriding/carburizing and plasma source low-energy ion enhanced deposition of thin films, for surface engineering of metallic materials was emerged as low-temperature, low-pressure surface modification technique. Plasma source ion nitriding onto AISI 316L austenitic stainless steel produced a high nitrogen face-centered-cubic phase (γ_N) layer about 10 μm thick at the temperature of 380 °C during 4 h with the high microhardness of HK_0.1 N 22.0 GPa. The microhardness of the nitrided surface from the titanium nitride phase [(Ti, Al, V)N] layer on Ti6Al4V alloy at 750 °C during 4 h achieved up to about HK_0.1 N 15.5 GPa. No pitting corrosion in the Ringer’s solution at 37 °C was detected by electrochemical polarization measurement for the nitrided AISI 316L stainless steel and Ti6Al4V alloy, respectively. Plasma source ion nitriding of the metallic materials provided the engineering surfaces with combined improvement in hardness and corrosion resistance.     

Anomalous conductivity and microstructure in gadolinium doped ceria prepared from nano-sized powder

The temperature and the oxygen partial pressure dependences of the electron and hole conductivities were measured by the dc polarization method using a Hebb–Wagner's ion blocking cell for Gd_0.2Ce_0.8O_1.9 polycrystalline bodies with grain size of 0.5 μm prepared by sintering of nano-sized powder. A significant enrichment of gadolinium was observed in the vicinity of the grain boundary by TEM/EDS analyses. The electron conductivity were comparable with those of conventional Gd_0.2Ce_0.8O_1.9 polycrystalline body with grain size of 2 μm, and it followed p(O₂)^− 1/4 dependence at temperatures T = 973–1273 K. However, the observed hole conductivity was higher than that of conventional Gd_0.2Ce_0.8O_1.9, and it did not follow p(O₂)^1/4 dependence. This anomalous p(O₂) dependence disappeared after the sample was treated at T = 1773 K for 38 h and grain size was enlarged to 2–10 μm.     

Thermoelectric properties in p-type nanostructured Ge-doped Sb100GeTe150 alloy

Ge-doped Sb₁₀₀GeTe₁₅₀ alloy were prepared using spark plasma sintering technique, and its thermoelectric properties were evaluated over the temperature range 318–492 K. Through XRD analysis, we observed the same single phase as Sb₂Te₃ and weakened diffraction peaks. Rietveld refinement reveals that there is 0.96 at.% Ge that occupies in the Sb sites, leading to the lattice distortion in the Sb–Te crystal. High-resolution TEM images show that there are many nanodomains randomly distributed in the matrix with a large amount of amorphous phase adjoined. Measurements indicated that the Seebeck coefficients (α) increase and the electrical and thermal conductivities decrease with temperature in the entire temperature range. The maximum α value reaches 135 μV/K at 492 K, and the thermal conductivities are about 0.3 W/mK lower than those of present Sb₂Te₃ for the corresponding temperatures. The highest thermoelectric figure of merit ZT for the nanostructured alloy Sb₁₀₀GeTe₁₅₀ is 0.84 at 492 K, whereas that of the currently prepared Sb₂Te₃ is 0.74 at the corresponding temperature.     

Synthesis,structure and magnetic entropy change of polycrystalline La1−xKxMnO3+δ

The use of a sol–gel synthetic method allows the preparation, at temperatures as low as 873 K, of single-phase perovskites in the potassium-doped lanthanide manganites La_1−xK_xMnO_3+δ. Samples prepared at 1273 K remain single phase and are constituted by submicrometer homogeneous particles, without deviation from nominal stoichiometries upon heating. These materials exhibit paramagnetic-to-ferromagnetic phase transitions at 230, 283, 338, and 344 K for x=0.075, 0.10, 0.165, and 0.20, respectively. By measuring the sample magnetization as a function of field and temperature we have determined the magnetic entropy change associated with these transitions. It is suggested by the results that these materials can be utilized as suitable magnetic refrigerants with very large temperature span.     

Ionic and electronic conductivities,stability and thermal expansion of La10 − x(Si,Al)6O26 ± δ solid electrolytes

Apatite-type La_10 − xSi_6 − yAl_yO_{27 − 3x/2 − y/2} (x = 0–0.33; y = 0.5–1.5) exhibit predominant oxygen ionic conductivity in a wide range of oxygen partial pressures. The conductivity of silicates containing 26.50–26.75 oxygen atoms per formula unit is comparable to that of gadolinia-doped ceria at 770–870 K. The average thermal expansion coefficients are (8.7–10.8) × 10^− 6 K^− 1 at 373–1273 K. At temperatures above 1100 K, silicon oxide volatilization from the surface layers of apatite ceramics and a moderate degradation of the ionic transport with time are observed under reducing conditions, thus limiting the operation temperature of Si-containing solid electrolytes.     

The influence of oxygen on the growth of silver on Cu(110)

The influence of the (2 × 1)O reconstruction on the growth of Ag on a Cu(110) surface was studied by scanning tunneling microscopy (STM) and Auger electron spectroscopy (AES). On the bare Cu(110) surface, Stranski–Krastanov growth of silver is observed at sample temperatures between 277 K and 500 K: The formation of a Ag wetting layer is followed by the growth of three-dimensional Ag wires. In contrast, on the oxygen-precovered Cu(110) surface, the growth of silver depends heavily on the substrate temperature. Upon Ag deposition at room temperature, a homogeneous, polycrystalline Ag layer is observed, whereas at 500 K, three-dimensional wires separated by (2 × 1)O reconstructed areas are formed. The behavior of a deposited Ag layer upon annealing is also influenced greatly by the presence of oxygen. On the bare surface, annealing does not change the Ag wetting layer and gives rise to Ostwald ripening of the Ag wires. On the oxygen-precovered surface, however, the initial polycrystalline Aglayer first transforms into Ag wires at around 500 K. Above this temperature, the depletion of the (2 × 1)O reconstructed areas due to Ag-induced O desorption is balanced by the formation of a Ag wetting layer. On both, the bare and the oxygen-precovered Cu(110) surface, the deposited silver diffuses into the Cu bulk at temperatures above 700 K.     

Specific heat of TbMn2(H,D)2

Specific heat (SH) measurements on TbMn₂(H,D)₂ powders have been performed in the temperature range from 2 to 350 K, in zero magnetic field and in 9 T. Due to the low heat conductivity of the samples, the measurements were carried out on a mixed Cu- and sample-powder pellet. For TbMn₂, the anti-ferromagnetic phase transition was manifest by a single SH peak at T_N=47 K, whereas a double SH peak at 281 and 288 K and an upturn below 5 K were observed for the hydride sample. Upon applying the magnetic field of 9 T, the SH upturn was suppressed, whereas no visible influence was found on the specific heat in the whole temperature range above 10 K as well as on the double peak.     

Effects of manganese and sulfur contents and slab reheating temperatures on the magnetic properties of non-oriented semi-processed electrical steel sheet

The effects of manganese and sulfur contents and slab reheating temperatures (SRTs) on the magnetic properties of non-oriented semi-processed electrical steel sheets were investigated. The core loss W15/50 of the steels increases with an increase of sulfur content in each steel with different manganese contents, while, the magnetic induction B50 hardly changed with an increase of the sulfur content at any manganese level. The SRTs affect the core loss in steels without hot band annealing, and in steels processed at an SRT of 1273 K showed the lowest core loss. Steels with higher sulfur content processed at an SRT of 1523 K showed deterioration of the core loss caused by the retardation of the grain growth at the recrystallization annealing by the fine MnS (ca.0.1 μm in diameter).     

Ionic conductivity of brownmillerite-type calcium ferrite under oxidizing conditions

The thermogravimetric and Mössbauer spectroscopy studies showed that, at atmospheric oxygen pressure, the oxygen content in Ca₂Fe₂O₅ brownmillerite is very close to stoichiometric at 300–1270 K. The orthorhombic lattice of calcium ferrite undergoes a transition from primitive (space group Pnma) to body-centered (I2mb) at 950–1000 K, which is accompanied with decreasing thermal expansion coefficient (TEC) and increasing activation energy for the total conductivity, predominantly p-type electronic. The steady-state oxygen permeation through dense Ca₂Fe₂O₅ ceramics is limited by the bulk ionic conduction. The ion transference numbers in air vary in the range 0.002–0.007 at 1123–1273 K, increasing with temperature. Analysis of stereological factors, which may affect oxygen diffusivity, suggests a dominant role of the ion jumps along octahedral and, possibly, tetrahedral layers of the brownmillerite structure. The ionic conductivity of calcium ferrite is higher than that of Ca₂FeAlO_5+δ, but lower compared to the oxygen-deficient perovskite phases based on SrFeO_3−δ where the diffusion pathways form a three-dimensional network. The average TECs of Ca₂Fe₂O₅ ceramics, calculated from dilatometric data in air, are 13.1 × 10^− 6 K^− 1 at 370–950 K and 11.3 × 10^− 6 K^− 1 at 970–1270 K.     

Effect of Cr substitution on the superconducting and magnetic properties of RuSr2Eu1.5Ce0.5Cu2O10−δ

In this paper we investigate the properties of polycrystalline series of Ru_1?xCr_xSr₂Eu_1.5Ce_0.5Cu₂O_10?δ (0.0 ? x ? 0.40) by resistivity, XRD and dc magnetization measurements. EuRu-1222 is a reported magneto superconductor with Ru spins magnetic ordering at temperatures near 100 K and superconductivity occurs in Cu–O₂ planes below T_c ? 40 K. The exact nature of Ru spins magnetic ordering is still being debated and no conclusion has been reached yet. In this work, we found the superconducting transition temperature T_c = 20 K from resistivity and dc magnetization measurements for pristine sample. DC magnetization measurements exhibited ferromagnetic like transition for all samples.