Optical and thermal properties of crystalline Tb: KLu(WO4)2

A single crystal of Tb: KLu(WO₄)₂ with dimensions of 40 mm × 40 mm × 18 mm has been grown by the top-seeded solution growth (TSSG) method. The color of the crystal is brown. Absorption and fluorescence spectra were measured at room temperature. The measured specific heat is a little lower than that of Yb: KLW (0.365 J/g K) at 90 °C. The measured mean linear coefficients of thermal expansion are α_a = 17.1643 × 10^− 6 K^− 1_, α_a^⁎ = 14.0896 × 10^− 6 K^− 1, α_b = 8.7938 × 10^− 6 K^− 1, α_c = 23.1745 × 10^− 6 K^− 1, α_c^⁎ = 20.2866 × 10^− 6 K^− 1. The results indicate that the crystal has a large anisotropy. The refractive index was measured.     

Preparation,characterization, thermal and third-order nonlinear optical properties of bis(tetraethylammonium)bis(2-thioxo-1,3-dithiole-4,5-dithiolato)cuprate(II)

The preparation and characterization of bis(tetraethylammonium)bis(2-thioxo-1,3-dithiole-4,5-dithiolato)cuprate(II), (I), are described. The thermal stability and thermal decomposition of (I) are studied both in air and under nitrogen flux. The nonlinear optical properties of (I) at 532 and 1064 nm are investigated by using the Z-scan technique with pulses of picoseconds duration. (I) exhibits self-defocusing effects at both wavelengths, strong saturable absorption at 532 nm and two-photon absorption at 1064 nm. The second molecular hyperpolarizability γ of (I) at 532 nm was estimated to be as high as 5.17 × 10^?31 esu. The origins have been analyzed and interpreted on the basis of crystal structure.     

Linear and non-linear optical properties of capped CdTe nanocrystals prepared by mechanical alloying

CdTe nanocrystals were prepared by mechanical alloying the elemental Cd and Te powders. The formation of CdTe with a single cubic phase after 20 h of ball milling was confirmed by X-ray diffraction (XRD). The surface of as-milled CdTe nanoparticles was then capped with polarization TOP/TOPO or (Na₃PO₄)_n organic ligand, which resulted in colorful dispersion solution with optical absorption peaks located at 573 nm and 525 nm, respectively. The third-order non-linearity, namely, the non-linear refraction and two-photon absorption (TPA) coefficient, of the capped CdTe dispersion samples were evaluated using Z-scan technique. The fitting of Z-scan experimental data with a special equation demonstrated that the capped CdTe nanocrystals possess large third-order susceptibilities at resonant wavelength. The non-linear figure of merit (γ/β) for 20 h as-milled CdTe nanocrystals after capping with TOP/TOPO was determined to be ∼ −2 × 10⁻⁵ m, which is nearly 215 times larger than the value reported for bulk CdTe crystals.     

Spectroscopic properties of HoAl3(BO3)4 single crystal

The Judd–Ofelt theory has been applied to analyze absorption spectra of Ho³⁺ ion in HoAl₃(BO₃)₄ measured in spectral range 300–700 nm at room temperature. The Judd–Ofelt spectroscopic parameters have been determined as: Ω₂ = 18.87 × 10⁻²⁰ cm², Ω₄ = 17.04 × 10⁻²⁰ cm², Ω₆ = 9.21 × 10⁻²⁰ cm². These parameters have been used to calculate radiative lifetimes and branching ratios of the luminescence manifolds. Three luminescent bands were found in the spectral range 450–700 nm ascribed to transitions from the ⁵F₅, (⁵F₄, ⁵S₂) and ³K₈ states to the ground state ⁵I₈. Experimental intensities of these luminescence transitions were compared with those calculated by using Judd–Ofelt theory and the system of kinetic equations for populations of starting luminescing states. Probabilities of radiativeless transitions were evaluated from this comparison.     

Biopolymer-clay nanoparticles composite system (Chitosan-laponite) for electrochemical sensing based on glucose oxidase

Nanocomposite matrix based on chitosan/laponite was successfully utilized to construct a new type of amperometric glucose biosensor. This hybrid material combined the merits of organic biopolymer, chitosan, and synthesized inorganic clay, laponite. Glucose oxidase (GOD) immobilized in the material maintained its activity well as the usage of glutaraldehyde was avoided. The composite films were characterized by Fourier transform infrared (FT-IR). The parameters affecting the fabrication and experimental conditions of biosensors were optimized. The sensitivity of the proposed biosensor (33.9 mA M^− 1 cm^− 2) permitted the determination of glucose in the concentration range of 1 × 10^− 6–5 × 10^− 5 M with a detection limit of 0.3 μM based on S/N = 3. The apparent Michaelis–Menten constant (K_M^app) for the sensor was found to be 15.8 mM.     

Oxygen partial pressure dependence of the structural properties of CdO thin films deposited by a modified reactive vacuum evaporation process

Thin films of cadmium oxide were thermally deposited on glass substrates at partial pressures of oxygen, pO₂ in the range 1.33×10⁻² to 0.133 Pa at a substrate temperature of 160 °C. Energy dispersive analysis of X-ray fluorescence (EDAX) revealed that the CdO films deposited at pO₂ value of 4.00×10⁻² Pa were nearly stoichiometric. X-ray diffractometry (XRD) confirmed the polycrystalline nature of the film structure. All the films showed an fcc structure of the NaCl-type, as the dominant phase. The films exhibited preferred orientation along the (1 1 1) diffraction plane. The texture coefficients calculated for the various planes at different oxygen partial pressures (pO₂) indicated that the maximum preferred orientation of the films occurred along the (1 1 1) plane at an oxygen partial pressure of 4.00×10⁻² Pa. This was interpreted in terms of oxygen chemisorption and desorption processes. The lattice parameters determined from the diffraction peaks were in the range 4.655–4.686 Å. The average lattice parameter a₀ found by extrapolation using the Nelson–Riley function was 4.696 Å. Both the lattice parameter and the crystallite size were found to increase with increased partial pressure of oxygen. On the other hand, the strain and dislocation density were found to decrease as the partial pressure of oxygen was raised. A maximum (80%) in the optical transmittance at λ=600 nm and minimum in the electrical resistivity (9.1×10⁻⁴ Ω cm) of the films occurred at an optimum partial pressure of oxygen of 4.00×10⁻² Pa. The results are discussed.     

Investigation on third order nonlinear optical,electrical and surface properties of organic stilbazolium crystal of 4-N,N-dimethylamino-N′-methylstilbazolium p-methoxybenzenesulfonate

The third order nonlinear optical, electric and dielectric properties of an organic stilbazolium derivative of 4-N,N-dimethylamino-N′-methylstilbazolium p-methoxybenzenesulfonate (DSMOS) crystal are reported. The nonlinear refractive index (n₂), two photon absorption coefficient (β) and third order optical susceptibility χ⁽³⁾ have been measured by Z-scan technique using Gaussian beam from the Nd:YAG laser at 1064 nm. The results show a large negative nonlinear refractive index (n₂ = −1.122 × 10−9 cm²/W) with a molecular two photon absorption coefficient β value of 3.625 × 10⁻⁶ cm/W. The low dielectric constant observed in the high frequency region indicates the suitability of the sample for electro-optic applications. The surface features are also investigated by atomic force microscopy (AFM).     

Negative thermal expansion in silicalite-1 and zirconium silicalite-1 having MFI structure

In situ high temperature X-ray diffraction (HTXRD) studies on monoclinic silicalite-1 (S-1, silica polymorph of ZSM-5) and an orthorhombic metallosilicate molecular sieve, zirconium silicalite-1 (ZrS-1) with MFI structure (Si/Zr = 50) have been carried out using a laboratory X-ray diffractometer with an Anton Parr HTK 1600 attachment. While the structure of the S-1 collapsed at 1123 K forming α-cristobalite. S-1 and ZrS-1 showed a complex thermal expansion behavior in the temperature range 298–1023 K, ZrS-1 was stable. Powder X-ray diffraction (PXRD) data taken in this region have shown strong negative lattice thermal expansion coefficient, α_V = −6.75 × 10⁻⁶ and −17.92 × 10⁻⁶ K⁻¹ in the temperature range 298–1023 K⁻¹ for S-1 and ZrS-1 samples, respectively. The thermal expansion behavior of S-1 and ZrS-1 is anisotropic, with the relative strength of contraction along a axis is more than that along b and c axes. Three different thermal expansion regions could be identified in the overall temperature range (298–1023 K) studied, corroborating with the three steps of weight loss in the TG curve of ZrS-1 sample. While the region between 298 and 423 K, displays positive thermal expansion coefficient with α_V = 2.647 × 10⁻⁶ and 4.24 × 10⁻⁶ K⁻¹, the second region between 423 and 873 K shows strong negative thermal expansion (NTE) coefficient α_V = −7.602 × 10⁻⁶ and −15.04 × 10⁻⁶ K⁻¹, respectively, for S-1 and ZrS-1 samples. The region between 873 and 1023 K, shows a very strong NTE coefficient with α_V = −12.08 × 10⁻⁶ and −45.622 × 10⁻⁶ K⁻¹ for S-1 and ZrS-1, respectively, which is the highest in the whole temperature range studied. NTE seen over a temperature range 298–1023 K could be associated with transverse vibrations of bridging oxygen atoms in the structure which results in an apparent shortening of the Si–O distances.     

Deposition and DC electrical characterisation of rf magnetron sputtered silicon nitride thin films

Silicon nitride (Si₃N₄) is an important insulator, frequently used in VLSI technology and for encapsulation. Conventionally it is prepared by low pressure and plasma-enhanced chemical vapour deposition, but may also be successfully deposited by RF sputtering. In the present work the sputtering process was characterised, together with some measurements on the high-field DC electrical properties in sandwich samples with Au electrodes. Films were Ar-sputtered using a Si₃N₄ sputtering target at gas pressures up to 2.12 Pa and RF discharge powers of 60–200 W. The deposition rate R was in the range 0.03–0.19 nm s^− 1 and was directly proportional to the discharge power and varied linearly with the pressure. Au electrodes formed sandwich structures with thicknesses of 50 nm–1 μm. Conductivity was essentially ohmic below 300 nm, while for the thicker films space-charge limited conductivity, dominated by an exponential distribution of traps, was observed. A mobility value of μ = 2.89 × 10^− 6 m² V^− 1 s^− 1 was derived from temperature measurements, and further analysis of the J–V data indicated a thermally generated electron concentration of 3.23 × 10¹⁹ m^− 3 and a trap concentration of 1.57 × 10²⁴ m^− 3. It was concluded that this method is suitable for the deposition of thin films, which have similar electrical properties to those prepared by chemical vapour deposition methods.     

A highly-sensitive l-lactate biosensor based on sol-gel film combined with multi-walled carbon nanotubes (MWCNTs) modified electrode

A new type of amperometric l-lactate biosensor based on silica sol-gel and multi-walled carbon nanotubes (MWCNTs) organic–inorganic hybrid composite material was developed. The sol-gel film was used to immobilize l-lactate oxidase on the surface of glassy carbon electrode (GCE). MWCNTs were used to increase the current response and improve the performance of biosensor. The sol-gel film fabrication process parameters such as H₂O : TEOS and pH were optimized, Effects of some experimental variables such as applied potential, temperature, and pH on the current response of the biosensor were investigated. Analytical characteristics and dynamic parameters of the biosensors with and without MWCNTs in the hybrid film were compared, and the results showed that analytical performance of the biosensor could be improved greatly after introduction of the MWCNTs. Sensitivity, linear range, limit of detection (S / N = 3) were 2.097 μA mM^− 1, 0.3 to 1.5 mM, 0.8 × 10^− 3 mM for the biosensor without MWCNTs and 6.031 μA mM^− 1, 0.2 to 2.0 mM, 0.3 × 10^− 3 mM for the biosensor with MWCNTs, respectively. This method has been used to determine the l-lactate concentration in real human blood samples.     

High-temperature electrical resistivity and heat capacity studies on nano-crystalline geikielite

We report here for the first time the temperature dependence of the electrical resistivity and heat capacity of nano-crystalline MgTiO₃ geikielite of up to 1000 K. The temperature dependence of heat capacity of nano-crystalline geikielite expressed as C_p = 46.44(5) + 0.0502(2)T − 4.56 × 10⁶T² + 1.423 × 10³T^− 0.5 − 8.672 × 10^− 6T^− 2, where C_p = is specific heat expressed in J/mol. K and T is the temperature in K. Both the electrical resistivity and heat capacity behaviour show that the geikielite (both the natural and synthetic nano-crystalline samples) are stable and remains electrically insulating up to 1000 K.     

Nonlinear optical properties of the PbS nanorods synthesized via surfactant-assisted hydrolysis

PbS nanorods were synthesized by surfactant-assisted homogenous hydrolysis. The products were characterized by UV–vis spectrophotometer, X-ray powder diffraction (XRD) and transmission electron microscope (TEM). PbS nanorods were measured by the Z-scan technique to investigate the third-order nonlinear optical (NLO) properties. The result of the NLO measurements shows that the PbS nanorods have the third-order nonlinear optical properties of both NLO absorption and NLO refraction with self-focusing effects. The nonlinear absorption coefficient and refractive index of the PbS nanorods are 2.16 × 10^− 9 m/W and 3.52 × 10^− 16 m²/W respectively.     

Studies on the electrochemical preparation of MgCeCo alloy thin films on Cu substrates in urea–DMSO system

Cyclic voltammetry was used to investigate the electrochemical behaviors of Mg(II), Ce(III) and Co(II) in 3.00 mol L^− 1 urea–DMSO (dimethylsulfoxide). The electrode processes of Mg(II), Ce(III) and Co(II) reducing on Pt electrodes were irreversible steps. The transfer coefficient of Mg(II), Ce(III) and Co(II) in 3.00 mol L^− 1 urea–DMSO system was calculated as 0.07, 0.05 and 0.05 at 298.15 K, respectively. The diffusion coefficient of Mg(II), Ce(III) and Co(II) in 3.00 mol L^− 1 urea–DMSO system was calculated as 2.27 × 10^− 10, 1.77 × 10^− 10 and 3.16 × 10^− 10 m² s^− 1 at 298.15 K, respectively. The MgCeCo alloy thin films with smooth, uniform and metallic luster were obtained on Cu substrates by cyclic electrodeposition in 0.01 mol L^− 1 Mg(ClO₄)₂–0.01 mol·L^− 1 Ce(CH₃SO₃)₃₋0.01 mol L^− 1 CoCl₂–3.00 mol L^− 1 urea–DMSO system. The potential sweep rate was found to be important with respect to the adhesion of the thin films.     

A novel iron (III)-PVC membrane potentiomeric sensor based on N-(2-hydroxyethyl)ethylenediamine-N,N',N"-triacetic acid

This work introduces a unique ionophore for the selective determination of Fe(III) ions. This ionophore was N-(2-hydroxyethyl)ethylenediamine-N,N′,N″-triacetic acid (NTA), presenting a high affinity towards the trivalent iron cations. The designed sensor exhibited a wide linear response with a slope of 19.5 ± 0.4 mV per decade over the concentration range of 1.0 × 10^− 9–1.0 × 10^− 2 mol L^− 1, while the illustrated detection limit was 3.0 × 10^− 10 mol L^− 1 of the Fe(III) ions concentration. It was concluded that the sensor response was pH independent in the range of 1.8–4.5. The sensor possessed the advantages of short conditioning time, fast response time (10 s) and, especially, good selectivity towards the transition and heavy metal ions as well as some mono, di and trivalent cations. Concerning the electrode lifetime, no considerable potential divergence was noticed for at least 10 weeks. The sensor accuracy was investigated in the potentiometric titration of a Fe(III) solution with EDTA.     

Spectroscopic properties of Tm3+/Al3+ co-doped sol–gel silica glass

Tm³⁺/Al³⁺ co-doped silica glass was prepared by sol–gel method combined with high temperature sintering. Glasses with compositions of xTm₂O₃–15xAl₂O₃–(100 − 16x) SiO₂ (in mol%, x = 0.1, 0.3, 0.5, 0.8 and 1.0) were prepared. The high thulium doped silica glass was realized. Their spectroscopic parameters were calculated and analyzed by Judd–Ofelt theory. Large absorption cross section (4.65 × 10⁻²¹ cm² at 1668 nm) and stimulated emission cross section (6.00 × 10⁻²¹ cm² at 1812 nm), as well as low hydroxyl content (0.180 cm⁻¹), long fluorescence lifetime (834 μs at 1800 nm), large σ_em × τ_rad (30.05 × 10⁻²¹ cm² ms) and large relative intensity ratio of the 1.8 μm (³F₄ → ³H₆) to 1.46 (³H₄ → ³F₄) emissions (90.33) are achieved in this Tm³⁺/Al³⁺ co-doped silica glasses. According to emission characteristics, the optimum thulium doping concentration is around 0.8 mol%. The cross relaxation (CR) between ground and excited states of Tm³⁺ ions was used to explain the optimum thulium doping concentration. These results suggest that the sol–gel method is an effective way to prepare Tm³⁺ doped silica glass with high Tm³⁺ doping and prospective spectroscopic properties.     

Compression behaviour and micro-structure evaluation of Zr57Nb5Cu15.4Ni12.6Al10 bulk metallic glass under high pressure

Compression behaviour and micro-structure evaluation of Zr₅₇Nb₅Cu_15.4Ni_12.6Al₁₀ bulk metallic glass is investigated at room temperature up to 32.8 GPa using in-situ high pressure energy dispersive X-ray diffraction with a synchrotron radiation source. The equation of state of the bulk metallic glass is − ΔV / V = 0.012P − 2.49 × 10^− 4P² − 9.5 × 10^− 7P³ + 5.02 × 10^− 8P⁴. The result shows that the nearest atom pair of the as-quenched bulk metallic glass corresponds to Zr–Zr correlations. And with pressure increasing, the nearest atom pair changes to a new one at 32.8 GPa.     

Effect of strain amplitude on the low-cycle fatigue behavior of a new Fe–15Mn–10Cr–8Ni–4Si seismic damping alloy

The low-cycle fatigue (LCF) properties and post-fatigue microstructure of a Fe–15Mn–10Cr–8Ni–4Si austenitic alloy were investigated under an axial strain control mode with total strain amplitudes, Δε_t/2, ranging from 2.5 × 10⁻³ to 2 × 10⁻². The fatigue resistance of the alloy was described by Coffin–Manson’s and Basquin’s relationships, and the corresponding fatigue parameters were evaluated. In addition, the Masing behavior, which is associated with a constant deformation mode during fatigue, was revealed at the examined strain amplitudes. Microstructural observations of the fatigue fractured samples showed that the strain induced ε-martensitic transformation accompanied by a planar slip of the Shockley partial dislocations in the austenite is the main deformation mode controlling the fatigue behavior of the studied alloy at Δε_t/2 < 2 × 10⁻². However, at Δε_t/2 = 2 × 10⁻², the formation of a cell structure was found in the austenite in addition to ε-martensitic transformation. The LCF resistance of the alloy was compared with conventional Cr–Ni austenitic stainless steels, ferrous base TRIP and TWIP steels and low yield point damping steels. It was found that at the studied strain amplitudes the alloy possessed a higher LCF resistance compared to conventional Fe-base alloys and steels. Remarkably, the fatigue ductility coefficient, ε_f′, of the studied alloy is 1.3–6 times higher than that of the stainless steels because of a cyclic deformation-induced ε-martensitic transformation. The results showed that the ε-martensitic transformation that occurred in the studied alloy during LCF is the main reason for the improved LCF resistance.     

Optical nonlinearities of BaTiO3 matrix-embedded Au nanoparticles

Composite thin films Au/BaTiO₃ comprising nanometer-sized gold particles embedded in BaTiO₃ matrices were synthesized on MgO(1 0 0) substrates by co-depositing Au and BaTiO₃ targets using pulsed laser deposition technique. The nanostructure of the films and the size distributions of the Au particles were analyzed by high-resolution transmission electron microscopy. Crystal lattice fringes from the Au nanocrystals and BaTiO₃ matrices were observed. The nonlinear optical properties of the Au/BaTiO₃ films were measured using z-scan method at the wavelength of 532 nm with a laser duration of 10 ns. The nonlinear refractive index n₂ and the nonlinear absorption coefficient β were determined to be 2.72 × 10⁻⁶ esu and −1.1 × l0⁻⁶ m/W, respectively.     

Growth and characterization of (Pb,La)TiO3 films with and without a special buffer layer prepared by RF magnetron sputtering

The (Pb, La)TiO₃ (PLT) ferroelectric thin films with and without a special buffer layer of PbO_x have been deposited on Pt/Ti/SiO₂/Si(100) substrates by RF magnetron sputtering technique at room temperature. The microstructure and the surface morphology of the films annealed at 600 °C for 1 h have been investigated by X-ray diffraction (XRD) and atomic force microscope (AFM). The surface roughness of the PLT thin film with a special buffer layer was 4.45 nm (5 μm × 5 μm) in comparison to that of 31.6 nm (5 μm × 5 μm) of the PLT thin film without a special buffer layer. Ferroelectric properties such as polarization hysteresis loop (P–V loop) and capacitance–voltage curve (C–V curve) of the films were investigated. The remanent polarization (P_r) and the coercive field (E_c) are 21 μC/cm² and 130 kV/cm respectively, and the pyroelectric coefficient is 2.75 × 10^− 8 C/cm² K for the PLT film with a special buffer layer. The results indicate that the (Pb, La)TiO₃ ferroelectric thin films with excellent ferroelectric properties can be deposited by RF magnetron sputtering with a special buffer layer.     

Development of an inconel self powered neutron detector for in-core reactor monitoring

The paper describes the development and testing of an Inconel600 (2 mm diameter×21 cm long) self-powered neutron detector for in-core neutron monitoring. The detector has 3.5 mm overall diameter and 22 cm length and is integrally coupled to a 12 m long mineral insulated cable. The performance of the detector was compared with cobalt and platinum detectors of similar dimensions. Gamma sensitivity measurements performed at the ⁶⁰Co irradiation facility in 14 MR/h gamma field showed values of −4.4×10⁻¹⁸ A/R/h/cm (−9.3×10⁻²⁴ A/γ/cm²-s/cm), −5.2×10⁻¹⁸ A/R/h/cm (−1.133×10⁻²³ A/γ/cm²-s/cm) and 34×10⁻¹⁸ A/R/h/cm (7.14×10⁻²³ A/γ/cm²-s/cm) for the Inconel, Co and Pt detectors, respectively. The detectors together with a miniature gamma ion chamber and fission chamber were tested in the in-core Apsara Swimming Pool type reactor. The ion chambers were used to estimate the neutron and gamma fields. With an effective neutron cross-section of 4b, the Inconel detector has a total sensitivity of 6×10⁻²³ A/nv/cm while the corresponding sensitivities for the platinum and cobalt detectors were 1.69×10⁻²² and 2.64×10⁻²² A/nv/cm. The linearity of the detector responses at power levels ranging from 100 to 200 kW was within ±5%. The response of the detectors to reactor scram showed that the prompt response of the Inconel detector was 0.95 while it was 0.7 and 0.95 for the platinum and cobalt self-powered detectors, respectively. The detector was also installed in the horizontal flux unit of 540 MW Pressurised Heavy Water Reactor (PHWR). The neutron flux at the detector location was calculated by Triveni code. The detector response was measured from 0.02% to 0.07% of full power and showed good correlation between power level and detector signals. Long-term tests and the dynamic response of the detector to shut down in PHWR are in progress.