X-ray diffraction study of Ba0.985Na0.015Ti0.985Nb0.015O3, Ba0.6Na0.4Ti0.6Nb0.4O3 and Ba0.3Na0.7Ti0.3Nb0.7O3 compositions

The Ba_0.985Na_0.015Ti_0.985Nb_0.015O₃, Ba_0.6Na_0.4Ti_0.6Nb_0.4O₃ and Ba_0.3Na_0.7Ti_0.3Nb_0.7O₃ compositions of the (1 − x) BaTiO₃–xNaNbO₃ (BTNNx) system have been studied by X-ray diffraction and by measurements of dielectric properties. The specimens with composition BTNN (x = 0.015, 0.40 and 0.70) have been refined by the JANA program from X-ray powder diffraction data. Ceramic samples with composition (1 − x) BaTiO₃ + xNaNbO₃ (where x = 0.015, 0.40 and 0.70) were prepared by calcinations from appropriate mixture of BaCO₃, TiO₂, Na₂CO₃ and Nb₂O₅. The calcined powder was sintered at temperature range 1200–1400 °C. As the composition x increased from 0.015 (and 0.70), the ferroelectric ceramics (x = 0.015, FE) with tetragonal phase changed to the ferroelectric relaxors (RFE, x = 0.40). RFE ceramics showed a peculiar diffuse phase transition and dielectric relaxation at the low temperature (down to 180 K) due to a frustration between RFE and FE state. These ceramics present the classical ferroelectric character when 0 ≤ x < 0.075 and 0.55 < x ≤ 1 and relaxor character when 0.075 ≤ x ≤ 0.55.     

Preparation of Ti–Al–Si alloys by reactive sintering

The isothermal section of the Dy–Co–Ti system at 500 °C has been investigated in the whole composition range by means of X-ray diffraction, thermal analysis, scanning electron microscopy and energy dispersive X-ray spectroscopy. The only ternary phase DyTi_xCo_12−x is of ThMn₁₂-type structure, space group I4/mmm, and shows a small homogeneity range of 1 ≤ x ≤ 1.6. The lattice parameters for DyTi_xCo_12−x with 1 ≤ x ≤ 1.56 are a = 0.8336(4)–0.8402(1) nm and c = 0.4691(3)–0.4727(1) nm. Along a constant Dy concentration, the solid solubilities of Ti in the compounds Dy₂Co₁₇, DyCo₃, DyCo₂ and Dy₃Co are about 2.0, 2.0, 3.0 and 4.0 at.%, respectively. The TiCo phase has a homogeneity range of 50–54 at.% Co at 500 °C and dissolves up to 2.0 at.% Dy.     

Synthesis of HCP, FCC and BCC structure alloys in the Mg–Ti binary system by means of ball milling

Mg_xTi_100−x (35 ≤ x ≤ 80) alloys with hexagonal close packed (HCP), face centered cubic (FCC) and body centered cubic (BCC) structures were successfully synthesized by means of ball milling. Mg_xTi_100−x alloys with a BCC structure at x = 35 and 50 and with a HCP structure at x = 80 were synthesized by milling of Mg and Ti powder using stainless steel milling balls and pots. At x = 65, the BCC and HCP phases were synthesized. Mg_xTi_100−x alloys with a FCC structure were synthesized at x = 35 and 50 by milling using zirconia milling balls and pots. The FCC and HCP phases were synthesized at x = 65 and 80 using zirconia milling balls and pots. The crystal structure of Mg_xTi_100−x alloys synthesized by the ball milling method depended on the materials of milling balls and pots. That indicates that milling products are determined by the dynamic energy given by the milling setup. The lattice parameters of Mg_xTi_100−x in the HCP, FCC and BCC phases increased with increase of the Mg content, x.     

Properties of Mn-doped FINEMET

Structural, thermodynamical and magnetic properties of Fe_73.5−xSi_13.5B₉Cu₁Nb₃Mn_x amorphous alloys, with Mn content x=1,3–15, were studied by means of X-ray diffraction (XRD), differential scanning calorimetry (DSC), Mössbauer spectroscopy (MS) and energy-dispersive X-rays (EDX), as-quenched and after annealing. The alloys with x≤7 suffer primary (above 550 °C) and secondary (below 680 °C) crystallisation, whereas the alloys with x≥9 only at 580 °C. Mn doping results in increase (for x≤7) and then (for x≥9) in decrease of grain size. The hyperfine field of the amorphous precursor and remainder substantially decrease with increase of Mn content x, whereas the fields in crystallites remain nearly independent of x. A paramagnetic component appears at x9 and grows with x.     

Subsolidus phase relations of the SrO–Ta2O5–CuO system at 900 °C in air

The subsolidus phase relations of the SrO–Ta₂O₅–CuO system were investigated in air. The samples were equilibrated at 900 °C. The ternary oxide Sr₃Ta₂CuO₉ compound is stable under these conditions. This phase presents a solid solution range, its actual composition being Sr₃Ta_2−xCu_1+xO_9+δ with 0.0 ≤ x ≤ 0.2. Up to about 5 at.% Cu can be incorporated in the Sr_3−xTa_1+xO_5.5+δ phase. Similarities with the SrO–Nb₂O₅–CuO system are discussed.     

Fabrication and study on Ni1−xFexO-YSZ anodes for intermediate temperature anode-supported solid oxide fuel cells

Bimetal oxides Ni_1−xFe_xO (x = 0.01, 0.04, 0.08, 0.1, 0.15, 0.2, 0.4, 0.5) were synthesized and studied as anodes for intermediate temperature solid oxide fuel cells (SOFCs) based on yttria-stabilized zirconia (YSZ) film electrolyte. A single cell consisted of Ni_1−xFe_xO-YSZ anode, YSZ electrolyte film, LSM–YSZ composite cathode was prepared and tested at the temperature from 600 °C to 850 °C with humidified hydrogen (75 ml min⁻¹) as fuel and ambient air as oxidant. It was found that the cell with Ni_0.9Fe_0.1O-YSZ anode showed the highest power density, 1.238 W cm⁻² at 850 °C, among the cells with different anode composition. The promising performance of Ni_1−xFe_xO as anode suggests that bimetal anodes are worth studied for SOFCs in future.     

Self-propagating high-temperature synthesis with post-heat treatment of La1−xSrxFeO3 (x = 0–1) perovskite as catalyst for soot combustion

La_1−xSr_xFeO₃ (x = 0–1) perovskite, Sr-substituted LaFeO₃, was prepared by Self-propagating high-temperature synthesis (SHS) and its catalytic activity for soot combustion was experimentally examined in comparison with that of a conventional Pt/Al₂O₃ catalyst. The products were also characterized by XRD, FE-SEM, and BET specific surface area. The XRD analysis revealed that all the products had a perovskite phase as the major compound, together with intermediate phases with higher x values (x = 0.7–1). The BET specific surface area of the products increased with x. Moreover, the catalytic activity for soot combustion also increased with x, wherein the BET specific surface area appeared an appropriate index for explaining the observed activity. The sample with x = 0.8 exhibited the highest activity for soot combustion among all the SHS products. The soot combustion temperature of this product was as much as 100 °C lower than that of non-catalytic soot combustion. In other words, it had the same activity as that at only 20 °C higher, in comparison to conventional Pt/Al₂O₃ catalyst. More significantly, average apparent activation energy of sample with x = 0.8 calculated by Friedman method using TG/DTA was approximately 15 kJ/mol lower than that of Pt/Al₂O₃ catalyst. This result suggested that La_1−xSr_xFeO₃ has the possibility to be an alternative catalyst to Pt/Al₂O₃ catalyst.     

A polyethylene glycol-assisted route to synthesize Pb(Ni1/3Nb2/3)O3-PbTiO3 in pure perovskite phase

Ferroelectric relaxors (1 − x)Pb(Ni_1/3Nb_2/3)O_3−xPbTiO₃ (PNN-PT) with a composition (x = 0.36) near the morphotropic phase boundary (MPB) were prepared by a polyethylene glycol (PEG)-assisted solid-state reaction route. PEG with a molecular weight of 200 was introduced during the ball milling process of the raw oxide powders. XRD and TG/DSC results demonstrated that the interaction between PbO and PEG favors the transformation of lead-rich pyrochlore to lead-deficient pyrochlore, thus facilitating the formation of perovskite phase. Consequently, pure perovskite powders were synthesized at a relatively low temperature of 850 °C. Ceramics fabricated with the PEG-assisted route show a room temperature dielectric constant of 4987 and a maximum dielectric constant (at T_max) of 24,307 at a frequency of 1 kHz. The piezoelectric constant d₃₃ measured was 460 pC/N.     

Thermal stability and primary phase of Al–Ni(Cu)–La amorphous alloys

Thermal stability and primary phase of Al_85+xNi_9−xLa₆ (x = 0–6) and Al₈₅Ni_9−xCu_xLa₆ (x = 0–9) amorphous alloys were investigated by X-ray diffraction and differential scanning calorimeter. It is revealed that replacing Ni in the Al₈₅Ni₉La₆ alloy by Cu decreases the thermal stability and makes the primary phase change from intermetallic compounds to single fcc-Al as the Cu content reaches and exceeds 4 at.%. When the Ni and La contents are fixed, replacing Al by Cu increases the thermal stability but also promotes the precipitation of single fcc-Al as the primary phase.     

Effect of Li2O on structure and optical properties of lithium bismosilicate glasses

Bismuth–silicate glasses containing lithium oxide having composition xLi₂O·(85 − x)Bi₂O₃·15SiO₂ (5 ≤ x ≤ 45 mol%) were prepared by melt quench technique. Density, molar volume and glass transition temperature for all the glass samples were measured. IR spectroscopy was used for structural studies of these glasses in the range from 400 to 1400 cm⁻¹. The increase of Li₂O content in glass matrix results in the decrease of the Si–O–Si bond angle and increase in the covalence nature of Bi–O bond. IR spectra suggest the presence of distorted [BiO₆] octahedral units and the degree of distortion increases with the addition of Li₂O in these glasses. The optical transmission spectra in the wavelength range from 200 to 3300 nm were recorded and optical band gap (E_g) was calculated. The values of E_g lie in between 2.81 and 2.98 eV. The values of average electronic oxide polarizability as well as optical basicity in these glasses were found to be dependent directly on Bi₂O₃/Li₂O ratio.     

Effects of Nb and C additions on the crystallization behavior, microstructure and magnetic properties of B-rich nanocrystalline Nd–Fe–B ribbons

The effects of Nb and C additions on the crystallization behavior, microstructure and magnetic properties of B-rich Nd_9.4Fe_79.6−xNb_xB_11−yC_y (x = 0, 2, and 4; y = 0, 0.5, and 1.5) alloy ribbons have been investigated. The results show that Nb and C additions change the crystallization behavior of Nd_9.4Fe_79.6B₁₁, avoid the formation of metastable Nd₂Fe₂₃B₃ phase, leading to the simultaneously precipitation of α-Fe and Nd₂Fe₁₄B phases. The results also show that Nb and C additions suppress the formation and growth of the soft α-Fe phases, leading to the presence of a large amount of Nd₂Fe₁₄B phases. Nb and C additions also refine the structure, and thus increase the exchange coupling interaction between the soft and hard phases. Excellent magnetic properties of B_r = 0.85 T, _iH_c = 1106 kA/m, and (BH)_max = 117 kJ/m³ have been achieved in Nd_9.4Fe_75.6Nb₄B_10.5C_0.5 alloy ribbons.     

Structural and magnetic susceptibility studies of samarium substituted magnesium–zinc ferrites

Polycrystalline soft ferrites Mg_1−x–Zn_x–Fe_2−y–Sm_y–O₄ (x = 0.0, 0.2, 0.4, 0.6, 0.8 and 1.0; y = 0.0, 0.05 and 0.1) were prepared by usual ceramic method. The samples were characterized by X-ray diffraction and IR techniques. Magnetic properties have been studied from magnetization and (a)–(c) susceptibility measurements. The XRD patterns of all the samples reveal the formation of single-phase cubic spinel. The IR spectra show two strong absorption bands in the frequency range 300–800 cm⁻¹. The magnetization measurements exhibit the Neel's collinear ferrimagnetic behavior for x ≤ 0.2 and suggest non-collinear Y–K (Yaffet–Kittel) type magnetic ordering for x ≥ 0.4. The samples with x ≥ 0.8 are paramagnetic at and above the room temperature. Variation of ac susceptibility with temperature exhibit the single domain structure (SD) with x = 0.0 and multi-domain (MD) structure with x ≥ 0.2 on substitution of Zn²⁺ content. On substitution of Sm³⁺ content, the samples exhibit SD for x = 0.0, MD for x = 0.2 and MD to SP transition for x ≥ 0.4.     

Substrates effect on Zn1−xMnxO thin films grown by RF magnetron sputtering

In this paper, we have presented the surface effect of the substrates on Mn doped ZnO (Zn_1−xMn_xO) thin films grown on Si(1 0 0) and sapphire [i.e. Al₂O₃(0 0 0 1)] by RF magnetron sputtering. These grown films have been characterized by X-ray diffraction (XRD), photoluminescence (PL) and vibrating sample magnetometer (VSM) to know its structural, optical and magnetic properties. All these properties have been found to be strongly influenced by the substrate surface on which the films have been deposited. The XRD results show that the Mn doped ZnO films deposited on Si(1 0 0) exhibit a polycrystalline nature whereas the films on sapphire substrate have only (0 0 2) preferential orientations indicating that the films are single crystalline. The studies of room temperature PL spectra reveal that the Zn_1−xMn_xO/Si(1 0 0) system is under severe compressive strain while the strain is almost relaxed in Zn_1−xMn_xO/Al₂O₃(0 0 0 1) system. It has been observed from VSM studies that Zn_1−xMn_xO/Al₂O₃(0 0 0 1) system shows ferromagnetic nature while the paramagnetic behaviour observed in Zn_1−xMn_xO/Si(1 0 0) system.     

Hydrogenation of CaLi2−xMgx (0 ≤ x ≤ 2) with C14 Laves phase structure

CaLi_2−xMg_x (0 ≤ x ≤ 2) which has the C14-type Laves phase structure has been successfully synthesized and hydrogenated. The C14-type Laves phase structure was kept after hydrogenation of CaLi_2−xMg_x (x = 0.2, 0.5, 1). After hydrogenation of CaLi₂ and CaMg₂, the Laves phase disappeared. The CaH₂ and LiH phases were formed from CaLi₂ and the CaH₂ and Mg phases from CaMg₂, respectively. CaLi_2−xMg_x (0 < x < 2) ternary alloys formed stable hydride phases with the C14-type Laves phase structure in contrast to CaLi₂ and CaMg₂ binary alloys.     

Wear-resistant Ti–B–N nanocomposite coatings synthesized by reactive cathodic arc evaporation

Wear-resistant Ti–B–N coatings have been synthesized by reactive arc evaporation of Ti–TiB₂ compound cathodes in a commercial Oerlikon Balzers Rapid Coating System. Owing to the strong non-equilibrium conditions of the deposition method, a TiN–TiB_x phase mixture is observed at low N₂ partial pressures, as determined by elastic recoil detection analysis, X-ray diffraction, X-ray spectroscopy, transmission electron microscopy and selected area electron diffraction. The indicated formation of a metastable solid solution of B in face-centered cubic TiN gives rise to a maximum in hardness (>40 GPa) and wear resistance on the expense of increased compressive stresses. A further saturation of the nitrogen content results in the formation of a TiN–BN nanocomposite, where the BN phase fraction was tailored by the target composition (Ti/B ratio of 5/3 and 5/1). However, the amorphous nature of the BN phase does not support self-lubricious properties, showing friction coefficients of 0.7 ± 0.1 against alumina. The effect of an increased bias voltage on structure and morphology was investigated from −20 to −140 V and the thermal stability assessed in Ar and air by simultaneous thermal analysis up to 1400 °C.     

Magnetic phase diagram of CrTe1−xSbx (0.0≤x≤1.0)

Measurements of the high field magnetization of CrTe_1−xSb_x (0.0≤x≤1.0) were carried out at 4.2 K in pulsed magnetic fields up to 300 kOe. The temperature dependence of the magnetization of CrTe_1−xSb_x was measured in the temperature range from 4.2 K to 800 K. The magnetic phase diagram of CrTe_1−xSb_x (0.0≤x≤1.0) was determined, which is similar to the typical one for the mixed crystals of the layered antiferromagnetic and ferromagnetic compounds proposed by de Gennes.     

Studies on structural and thermal expansion properties of Ho2−xLnxMo4O15 (Ln = Er, Sm and Ce) solid solutions

Three new series of Ho_2−xEr_xMo₄O₁₅ (x = 0.0–2.0), Ho_2−xSm_xMo₄O₁₅ (x = 0.0–0.6) and Ho_2−xCe_xMo₄O₁₅ (x = 0.0–0.25) solid solutions have been prepared successfully by solid-state reaction and studied by powder X-ray diffraction. All the XRD patterns of these molybdates can be indexed in monoclinic space group P2₁/c. Lattice parameters a, b and c of Ho_2−xLn_xMo₄O₁₅ decrease linearly with increasing erbium content and increase with increasing samarium or cerium content. Thermal expansion behaviors of Ho_2−xLn_xMo₄O₁₅ have been investigated in the 25–500 °C temperature range with high-temperature X-ray diffraction. The temperature dependence of Mo(2)–O14 interaction looks like to be responsible for their thermal expansion behaviors.     

Magnetic and structural properties of the chromium-based Mn1−xCdxCr2S4 thiospinel

The (Mn_1−xCd_x)Cr₂S₄ phases (0 ≤ x ≤ 0.6) have been synthesized from the corresponding elements at 1123 K. These samples were characterized by powder X-ray diffraction (XRD) and magnetic susceptibility. The (Mn_1−xCd_x)Cr₂S₄ compounds crystallize in the space group Fd-3m with cell parameters a = 10.101(6) Å, 10.139(3) Å, 10.165(2) Å, and 10.192(1) Å for x = 0, 0.2, 0.4 and 0.6, respectively. An overall ferrimagnetic behavior is observed for all samples. The ferromagnetic component increases rapidly when manganese is substituted by non-magnetic cadmium, as shown by ZFC/FC measurements. At the same time, the value of the magnetization M₅₀ at 50 kOe, deduced from M(H) loops, also increases with increasing cadmium content because the antiferromagnetic alignment between chromium and manganese spins is progressively lost, leading toward well aligned moments pointing into the same direction. These results are explained by a rearrangement of the chromium spins when Mn located at the tetrahedral sites, is substituted by Cd.     

Characterization of potassium lithium niobate (KLN) ceramic system

The room temperature stability region of the tetragonal tungsten bronze-type potassium lithium niobate (K₃Li₂Nb₅O₁₅, KLN) has been determined by X-ray phase analysis on ceramic samples synthesized by solid state reaction in the composition range of [K₂O] = 28–33 mol%, [Li₂O] = 12.5–20.5 mol% and [Nb₂O₅] = 50.5–55.5 mol%. Lattice parameters and temperature dependence of the dielectric constants were measured on single phase samples. The axial a/c ratio of the cell parameters, the density and the Curie temperature of the ferroelectric samples have been found predominantly characteristic for the Nb₂O₅ content, varying progressively between 3.11–3.14, 4.431–4.596 g/cm³ and 492–460 °C, respectively. The results are discussed from the points of view of defect chemistry and phase stability. The concentration of intrinsic defects formed primarily by antisite Nb atoms at Li sites has been estimated on the basis of “alkali cation vacancy formation model”.     

The crystal structure of HfZrP

The crystal structure of HfZrP has been determined using single crystal X-ray diffraction data. This compound crystallizes in the orthorhombic space group Cmmm (No.65), with a=19.004(3), b=29.372(4), c=3.565(1) Å and the Zr₂P structure type. The Hf and Zr atoms are disordered on one site with total occupancy of 1.0. X-ray powder patterns indicate that (Hf_xZr_1−x)₂P alloys consist of single phase (Zr₂P-type),two phases and single phase (Hf₂P-type) corresponding to 0≤x≤0.5, 0.5<x<0.8 and 0.8≤x≤1.0, respectively.