Characterization of silicon doped with sodium upon high-voltage implantation

The depth distribution profiles of sodium atoms in silicon upon high-voltage implantation (ion energy, 300 keV; implantation dose, 5 × 10¹⁴ and 3 × 10¹⁵ cm ^?2) are investigated before and after annealing at temperatures in the range T _ann = 300–900°C (t _ann = 30 min). Ion implantation is performed with the use of a high-resistivity p-Si (ρ= 3–5 kΩ cm) grown by floating-zone melting. After implantation, the depth distribution profiles are characterized by an intense tail attributed to the incorporation of sodium atoms into channels upon their scattering from displaced silicon atoms. At an implantation dose of 3 × 10¹⁵ ions/cm², which is higher than the amorphization threshold of silicon, a segregation peak is observed on the left slope of the diffusion profile in the vicinity of the maximum after annealing at a temperature T _ann = 600°C. At an implantation dose of 5 × 10¹⁴ ions/cm², which is insufficient for silicon amorphization, no similar peak is observed. Annealing at a temperature T _ann = 700°C leads to a shift of the profile toward the surface of the sample. Annealing performed at temperatures T _ann ≥ 800°C results in a considerable loss of sodium atoms due to their diffusion toward the surface of the sample and subsequent evaporation. After annealing, only a small number of implanted atoms that are located far from the region of the most severe damages remain electrically active. It is demonstrated that, owing to the larger distance between the diffusion source and the surface of the sample, the superficial density of electrically active atoms in the diffusion layer upon high-voltage implantation of sodium ions is almost one order of magnitude higher than the corresponding density observed upon low-voltage implantation (50–70 keV). In this case, the volume concentration of donors near the surface of the sample increases by a factor of 5–10. The measured values of the effective diffusion parameters of sodium at annealing temperatures in the range T _ann = 525–900°C are as follows: D ₀ = 0.018 cm²/s and E _a = 1.29 eV/kT. These parameters are almost identical to those previously obtained in the case of low-voltage implantation.     

EPR study of radiation-induced defects in carbonate-containing hydroxyapatite annealed at high temperature

Radiation-induced (γ or UV) paramagnetic defects in carbonate-containing hydroxyapatite (HAP) annealed at high (600–950 °C) temperature were studied by EPR. The complex spectra reveal the presence of different paramagnetic species. Their contributions were found to be strongly dependent on the annealing temperature as well as microwave power, thus, by the adjustment of experimental conditions some of the components can be eliminated that allowed to record EPR spectra caused by no more than two types of paramagnetic defects. All experimental spectra were analyzed using computer simulation. The parameters of the paramagnetic defects detected were determined, and the centers models were discussed. It was found that high-temperature annealing influences essentially the formation of radiation-induced defects in HAP. The СО₃³⁻, О⁻ centers and oxygen vacancy V_O⁻ were shown to be the main stable γ-induced defects in the HAP annealed at high temperatures. New paramagnetic defect with the parameters g_|| = 2.002, g_⊥ = 2.0135 was detected and tentatively identified as an O-related radical. The γ-induced EPR response from СО₃³⁻ radicals was found to be more intense than response from CO₂⁻ in non-annealed HAP. UV-irradiation was found to create smaller amounts of paramagnetic defects in comparison with γ-rays. Besides, oxygen vacancy V_O⁻ was not observed, while two other centers (СО₃⁻ and the center of unknown nature) appear in the UV-induced EPR spectra.     

Sequence of phase formation during solid-state synthesis in Al/Ni films (Al: Ni = 60: 40 at %)

The structure formed during solid-state synthesis in thin bilayer Al/Ni films with the ratio Al: Ni = 60: 40 (at %) has been investigated. The films were obtained by thermal evaporation in vacuum with a residual pressure of 10^?5–10^?6 Torr. Solid-state synthesis was performed by diffusion reaction. The sequence of phase formation upon vacuum annealing of bilayer Al/Ni films has been established: Al + Ni → Al₃Ni + Ni (T _ann = 180°C) → Al₃Ni₂ (T _ann = 220°C).     

Tailoring the exchange bias of Ni/NiO nanogranular samples by the structure control

The exchange bias (EB) effect has been studied in Ni/NiO nanogranular samples obtained by annealing in H₂, at selected temperatures (200≤T_ann≤300 °C), NiO powder previously milled for 5, 10, 20 and 30 h. Both the as-milled NiO powders and the Ni/NiO samples have been analyzed by X-ray diffraction and the exchange bias properties have been investigated in the 5-200 K temperature range. The structure and the composition of the Ni/NiO samples can be satisfactorily controlled during the synthesis procedure by varying both T_ann and the milling time of the precursor NiO powders. In particular, by increasing this last parameter, the mean grain size of the NiO phase reduces down to the final value of 16 nm and the microstrain increases, which is consistent with an enhancement of the structural disorder. The structure of the milled NiO matrix strongly affects the process of nucleation and growth of the Ni nanocrystallites induced by the H₂ treatments, so that, T_ann being equal, the amount and the mean grain size D_Ni of the Ni phase vary substantially in samples having different milling times. Such features of the Ni phase determine the extent of the Ni/NiO interface and consequently the magnitude of the exchange field H_ex: the highest value (∼940 Oe) has been measured at T=5 K in a sample containing ∼7 wt% Ni and with D_Ni=19 nm. However, in Ni/NiO samples with very different structural characteristics and different values of H_ex at T=5 K, the EB effect vanishes at the same temperature (∼200 K) and the same thermal dependence of H_ex is observed. We consider that the evolution of the EB effect with temperature is ultimately determined by the microstructure of the Ni/NiO interface, which cannot be substantially modified by changing the synthesis parameters, milling time and T_ann.     

NO 3 2− and CO 2 − centers in synthetic hydroxyapatite: Features of the formation under γ- and UV-irradiations

The EPR studies of synthetic hydroxyapatite containing carbonate and nitrate ions exposed to γ-ray and UV irradiations have been performed. It has been found that γ irradiation leads to the formation of both NO₃²⁻ and CO₂⁻ paramagnetic centers, while the UV irradiation induces only NO₃²⁻ centers. To explain this fact, the hypothesis has been proposed, according to which in the hydroxyapatites studied, there coexist complexes consisting of nitrate ions and shallow electron traps that serve as sources of secondary electrons during UV irradiation. The EPR spectroscopy parameters (g and A) of the detected centers have been determined and compared with similar centers in hydroxyapatite with a different impurity composition. The study of the thermal stability of the centers has demonstrated that, in the temperature range 20–300°C, the NO₃²⁻ centers formed by UV irradiation are more stable than the same centers created by γ-ray irradiation.     

Optimization of calcination temperature of lead-free BiFeO3–BaTiO3 high-temperature piezoceramics

0.7BiFeO₃-0.3BaTiO₃+1mol% MnO₂(0.7BFO-0.3BTO) ceramics were synthesized by conventional solid-state powder method under different calcination temperatures (T_cal) between 770 and 830 °C. The phase structure, microstructure, and ferroelectric and piezoelectric properties changed greatly depending on the applied T_cal. Benefitting from the formation of low defect levels and large grain size and an appropriate morphotropic phase boundary (MPB) with the rhombohedral-to-pseudocubic phase ratio = 49.1 : 50.9, BFO-BTO ceramics calcined at 785 °C showed the best ferroelectric, piezoelectric, and insulating properties (P_r = 23.1 μC/cm², E_C = 25.8 kV/cm, d₃₃ = 167.8 pC/N, k_p = 0.342%). Above T_cal = 800 °C, however, the ferroelectric and piezoelectric properties deteriorated because volatilization of Bi and reduction of Fe caused a poor insulating property and high degree of chemical inhomogeneity. Moreover, the ceramics calcined at 785 °C showed a high Curie temperature (T_C) of 509.2 °C and excellent thermal aging resistance of d₃₃ up to 450 °C, demonstrating great potential for use in high-temperature applications.     

Structural and optical characterization of sol–gel derived Tm-doped BaTiO3 nanopowders and ceramics

Nanocrystalline Tm³⁺(5%)-doped BaTiO₃ (BT-Tm) has been synthesized by the sol–gel method. The morphology, structure, and optical properties of powders and ceramics were characterized. The average grain size of the gel precursor annealed at 700 and 900 °C was 20 nm and 30 nm, respectively. These powders were single phase and crystallized with a cubic structure while the BT-Tm sintered ceramics were crystallized with the tetragonal BaTiO₃ structure. The photoluminescence spectra showed typical transitions of Tm³⁺ ions and a structure consistent with the Tm³⁺ ions incorporation in the BaTiO₃ crystalline lattice. Thermoluminescence peaks recorded at 300 °C (for annealed samples) or at 230 °C for the ceramic sample were assigned to the recombination of the Tm²⁺-electron traps located mainly at the surface of the nano-crystals or inside the microcrystals, respectively.     

Electrical conductivity of fully densified nano CaZr0.90In0.10O3 − δ ceramics prepared by a water-based gel precipitation method

Water-based gel precipitation method was first applied to synthesize high purity nano CaZr_0.90In_0.10O_3 ? δ powders suitable for fabricating dense ceramics at lower temperature. By using CaCO₃, Zr(NO₃)₄ and In(NO₃)₃ as raw materials, PEG as dispersant, CaZr_0.90In_0.10O_3 ? δ with an average particle size of about 40 nm was obtained at 850 °C, which was nearly 350 °C lower than that of traditional solid-state reaction method. Fully densified ceramics with an average grain size of 200–300 nm were obtained at 1350 °C, a temperature about 250 °C lower than that of traditional sintering techniques. Experimental results showed that the flexure stress, total, bulk and grain boundary protonic conductivities of the ceramics were more favorable than those of the ceramics fabricated at 1500 °C and 1600 °C from the powders synthesized by solid-state reaction method.     

An influence of deposition temperature on structural,optical and electrical properties of sprayed ZnO thin films of identical thickness

Nanocrystalline ZnO thin films were deposited at different temperatures (T_s = 325 °C–500 °C) by intermittent spray pyrolysis technique. The thickness (300 ± 10 nm) independent effect of T_s on physical properties was explored. X-Ray diffraction analysis revealed the growth of wurtzite type polycrystalline ZnO films with dominant c-axis orientation along [002] direction. The crystallite size increased (31 nm–60 nm) and optical band-gap energy decreased (3.272 eV–3.242 eV) due to rise in T_s. Scanning electron microscopic analysis of films deposited at 450 °C confirmed uniform growth of vertically aligned ZnO nanorods. The films deposited at higher T_s demonstrated increased hydrophobic behavior. These films exhibited high transmittance (>91%), low dark resistivity (～10^?2 Ω-cm), superior figure of merit (～10^?3 Ω^?1) and low sheet resistance (～10² Ω/□). The charge carrier concentration (η -/cm³) and mobility (μ – cm²V^?1s^?1) are primarily governed by crystallinity, grain boundary passivation and oxygen desorption effects.     

Radiation-induced defects in annealed carbonate-containing hydroxyapatite

The effect of preliminary (before irradiation) annealing of synthetic carbonate-containing hydroxyapatite powders on the formation of paramagnetic centers under γ-ray and ultraviolet irradiation has been investigated. Annealing of the samples has been performed in the temperature range from 100 to 700°C. It has been found that electron paramagnetic resonance spectra of radiation-induced defects depend substantially on the annealing temperature. The paramagnetic centers CO ₂ ^? dominate in the samples annealed to 250°C (γ-ray irradiation) and 500°C (ultraviolet irradiation). In the samples annealed above 400°C, other defects, in particular, the O^? and CO ₃ ^3? centers, play a significant role. Annealing at some temperatures leads to an increase in the radiation sensitivity of the material. The observed effects can be associated with the escape of molecular water from the annealed hydroxyapatite samples and with the corresponding transformation of the defect subsystem of the material.     

Polymorphic phase transition and thermal stability in squaric acid (H2C4O4)

Phase transformations in squaric acid (H₂C₄O₄) have been investigated by thermogravimetry and differential scanning calorimetry with different heating rates β. The mass loss in TG apparently begins at onset temperatures T_di=245±5 °C (β=5 °C min^?1), 262±5 °C (β=10 °C min^?1), and 275±5 °C (β=20 °C min^?1). A polymorphic phase transition was recognized as a weak endothermic peak in DSC around 101 °C (T_c⁺). Further heating with β=10 °C min^?1 in DSC revealed deviation of the baseline around 310 °C (T_i), and a large unusual exothermic peak around 355 °C (T_p), which are interpreted as an onset and a peak temperature of thermal decomposition, respectively. The activation energy of the thermal decomposition was obtained by employing relevant models. Thermal decomposition was recognized as a carbonization process, resulting in amorphous carbon.     

Enhanced piezoelectric properties near the morphotropic phase boundary in lead-free (1-x)(Bi0.5K0.5)TiO3-xBi(Ni0.5Ti0.5)O3 ceramics

Lead-free piezoelectric ceramics of the composition (1-x)(Bi_0.5K_0.50)TiO₃-xBi(Ni_0.50Ti_0.50)O₃ or (1-x)BKT-xBNiT (when x = 0–0.20 mol fraction) were prepared by a conventional mixed-oxide method and sintered at 1050 °C for 4 h. The effects of BNiT content on the phase equilibria, and the dielectric, ferroelectric and piezoelectric properties were systematically investigated. High density sintered specimens (5.71–6.12 g/cm³) were obtained for all compositions. X-ray diffraction patterns showed that all BKT-BNiT samples exhibited a single perovskite phase which confirms that BNiT and BKT formed a solid solution up to x = 0.20. A morphotropic phase boundary (MPB) separating a BKT-rich tetragonal phase and a BNiT pseudo-cubic phase was identified over the compositional range 0.05 < x < 0.10, where enhanced electrical properties were observed. The optimum dielectric properties (ε_r = 1710, tanδ = 0.036), ferroelectric properties (P_r = 16.6 μC/cm², E_c = 22.5 kV/cm and R_sq = 0.86) and piezoelectric properties (d₃₃ = 288 pC/N, S_max = 0.22% and d^*₃₃ = 313 pm/V) were observed with a relatively high T_m ∼ 304 °C within this MPB region. Overall, these results indicate that the BKT-BNiT ceramic system is a promising lead-free piezoelectric candidate for further development for actuator applications.     

Enhanced ferroelectric,piezoelectric and dielectric properties of (1-x)CaBi2Nb2O9-xBaZr0.2Ti0.8O3 high-temperature piezoelectric composite ceramics

Among Aurivillius layer-structured materials, CaBi₂Nb₂O₉ is a best potential candidate for ultrahigh-temperature applications because of its highest Curie temperature of about 940 °C. In this paper, (1-x)CaBi₂Nb₂O₉-xBaZr_0.2Ti_0.8O₃ composite ceramics were prepared by conventional solid-state sintering method. The dielectric results show that the introduction of BaZr_0.2Ti_0.8O₃ not only increases the permittivity of the material, but also reduces its dielectric loss. The optimum electrical properties were obtained in the x = 0.01 sample with piezoelectric coefficient (d₃₃) of 15.1 pC/N and high ferroelectric remnant polarization (P_r) of 9.9 μC/cm². Furthermore, the composite samples show good thermal depoling performance, the d₃₃ of the x = 0.01 sample is 13.8 pC/N, which is about 91% of the initial value after depoling at 800 °C. Therefore, (1-x)CaBi₂Nb₂O₉-xBaZr_0.2Ti_0.8O₃ is one of the candidates for high temperature piezoelectric materials.     

Conductivities of electrolytes based on PEI-b-PEO-b-PEI triblock copolymers with lithium and copper TFSI salts

Tri block-copolymer poly(iminoethylene)-b-poly(oxyethylene)-b-poly(iminoethylene) with a poly(oxyethylene) central block (PEI-b-PEO-b-PEI) were used as a “dual” matrix for polymer electrolytes having selectivity for hard cations (Li⁺/PEO) in one phase and for soft cations (Cu²⁺/PEI) in the other. Conductivity measurements were recorded for 20:1, 12:1 and 8:1 coordinating atom (O or/and N) to cation (Li⁺, Cu²⁺) ratios, for each of the three complexes studied: PEI-b-PEO-LiTFSI-b-PEI, PEI-Cu(TFSI)₂-b-PEO-b-PEI-Cu(TFSI)₂ and PEI-Cu(TFSI)₂-b-PEO-LiTFSI-b-PEI-Cu(TFSI)₂. For either low (20 °C) or high temperature (80 °C) the highest conductivity was given by the polymer electrolyte based on Cu(TFSI)₂ with N/Cu²⁺ = 20:1 (10^− 6, respectively 2 × 10^− 4 S cm^− 1). In the present paper, the conductivity evolution is discussed in relation with the polymer structure, the type and the concentration of the salt and the thermal behavior of our systems.     

Basic thermoluminescent and dosimetric properties of Al2O3:C irradiated by pulse intensive electron beam

The effect of deep traps filled by a pulse electron beam on the thermoluminescent (TL) properties in Al₂O₃:C dosimetric crystals is studied. When the deep traps are filled, the dosimetric peak at 170 °C acquires a double-peak structure not present in the initial samples. The effect of the population of the deep centers having various nature (electron or hole traps) and energy depth on the shape of the dosimetric TL peak structure is analyzed. An assumption is made that in the temperature ranges of 350–500 °C and 650–750 °C, electron traps are emptied, whereas at T = 500–650 °C hole traps are emptied. The possibility of using the TL associated with deep traps in high-dose dosimetry of pulse electron beams is shown.     

Synthesis and characterization of nanocrystalline HAp powders prepared by using aloe vera plant extracted solution

Nanocrystalline hydroxyapatite (HAp) powders were synthesized by a simple method using aloe vera plant extracted solution. To obtain nanocrystalline HAp, the prepared precursor was calcined in air at 400–800 °C for 2 h. The phase composition of the calcined samples was studied by X-ray diffraction (XRD) technique. The XRD results confirmed the formation of HAp phase. With increasing calcination temperature, the crystallite of the HAp increased, showing the hexagonal structure of HAp with the lattice parameter, a, in a range of 0.9520–0.9536 nm and c of 0.6739–0.6928 nm. The particle sizes of the powder were obtained to be 43–171 nm. The optical properties of the calcined powders were characterized by Raman and FTIR spectroscopies. The Raman spectra showed a main peak of the phosphate vibration mode (ν₁(PO₄)) at ∼963 cm⁻¹ for all the calcined samples. The peaks of the phosphate carbonate and hydroxyl vibration modes were observed in the FTIR spectra for all the calcined powders. The morphology tends to change from a spherical shape to a rod-like shape with increasing calcination temperature as revealed by TEM.     

Thermoluminescence and optically stimulated luminescence characteristics of Al2O3 doped with Tb

In the present work policrystals of α − Al₂O₃ doped with terbium were synthesized using the solvent evaporation method. The samples were prepared using Al(NO₃)₃·9H₂O and Tb(NO₃)₃·5H₂O reagents, with Tb concentrations between 1 and 5 mol% and thermally treated at high temperature above ∼1400 °C. X-ray diffraction measurements showed the α-phase formation of samples. TL glow curve presented an intense peak at ∼190 °C and two other with low intensity at 290 and 350 °C after gamma irradiation. The best doping concentration which presented high luminescence was the sample doped with 3 mol% of Tb. TL spectra and fluorescence measurements showed similar luminescence spectra with lines attribute to Tb³⁺ ions. A linear behavior to gamma dose between 1 and 20 Gy was observed in TL, using 190 °C peak as well as in OSL signal, this last carried out using 532 nm wavelength stimulation.     

Thermal expansion behavior and chemical compatibility of BaxSr1−xCo1−yFeyO3−δ with 8YSZ and 20GDC

Perovskite oxides of the composition Ba_xSr_1−xCo_1−yFe_yO_3−δ(BSCF) were synthesized via a modified Pechini method and characterized by X-ray diffraction, dilatometry and thermogravimetry. Investigations revealed that single-phase perovskites with cubic structure can be obtained for x ≤ 0.6 and 0.2 ≤ y ≤ 1.0. The as-synthesized BSCF powders can be sintered in several hours to nearly full density at temperatures of over 1180 °C. Thermal expansion curves of dense BSCF samples show nonlinear behavior with sudden increase in thermal expansion rate between about 500 °C and 650 °C, due mainly to the loss of lattice oxygen caused by the reduction of Co⁴⁺ and Fe⁴⁺ to lower valence states. Thermal expansion coefficients (TECs) of BSCF were measured to be 19.2–22.9 × 10^− 6 K^− 1 between 25 °C and 850 °C. Investigations showed further that Ba_0.5Sr_0.5Co_0.8Fe_0.2O_3−δ is chemically compatible with 8YSZ and 20GDC for temperatures up to 800 °C, above which severe reactions were detected. After being heat-treated with 8YSZ or 20GDC for 5 h above 1000 °C, Ba_0.5Sr_0.5Co_0.8Fe_0.2O_3−δ was completely converted to phases like SrCoO_3−δ, BaCeO₃, BaZrO₃, etc.     

Magnetic properties and magnetic entropy changes of perovskite manganese oxide La0.8-xEuxSr0.2MnO3 (x = 0, 0.075)

Magnetocaloric effect and critical exponent analysis of La_0.8-xEu_xSr_0.2MnO_{3 (}x = 0, 0.075) manganites synthesized via a solid state reaction route have been explored. Rietveld analysis indicates that crystal structure of La_0.8-xEu_xSr_0.2MnO_{3 (}for x = 0.0) is in orthorhombic structure with pbnm space group. After the substitution of Eu, the structure changes from orthorhombic (for x = 0.0) to rhombohedral structure for (x = 0.075) with $\mathrm{R}\overline{3}c$ space group. The T_C is 287 K and 271 K for the samples with x = 0.000 and x = 0.075, respectively, and the magnetic entropy change is 2.76J K ^− 1•kg⁻¹ for x = 0.000 and 3.94J K ^− 1•kg⁻¹ for x = 0.075. The real cooling power (RCP) is 447.7 J•kg⁻¹ for the sample with x = 0.000 and 445 J•kg⁻¹ for the samples with x = 0.075. Both samples show a second order phase transition in the vicinity of T_C. The critical exponents were determined using modified Arrott plots and Kouvel-Fisher methods. The critical behavior of these two samples fit best with the mean field model.     

Low-temperature preparation and properties of ceramics with composition (1−x)CaTiO3−xPbF2−xLiF

Fluorinated ceramics with initial composition (1−x)CaTiO₃+xPbF₂+xLiF were sintered at 950 °C. The X-ray diffraction (XRD) patterns of the samples showed the formation of a novel solid solution in the initial composition range 0⩽x⩽0.125. SEM observations were performed on fractured ceramics and DSC analyses were carried out from room temperature up to 600 °C. Three second-order phase transitions were detected for all the samples. Capacitors were prepared from the pre-sintered ceramics then dielectric measurements were performed as a function of temperature in the frequency range 10²–4×10⁷ Hz. The ε′_r−T curves exhibit the profile of dielectrics for class I capacitors, however the values of tan δ are too high (tan δ⩾1%).