Experimental and theoretical studies on bis(glycine) lithium nitrate (BGLiN): A physico-chemical approach

Good quality and bulk size single crystal (size: 20×13×8 mm³) of bis(glycine) lithium nitrate (BGLiN) was grown by a slow evaporation solution technique from the aqueous solutions at constant temperature i.e. 27 °C using synthesized materials. Crystal system and lattice parameters were determined by single crystals as well as powder X-ray diffraction analysis. The lattice parameters of the titled compound are a=10.0223 Å, b=5.0343 Å, c=17.0510 Å, and V=860.312 Å³ and it crystallized in an orthorhombic system with space group Pca2₁ obtained by single crystal XRD. Elemental composition was confirmed by energy dispersive X-ray spectroscopic analysis. Optical absorption spectrum was recorded and various optical parameters such as optical transmission (~60%), and optical band gap (4.998 eV) were calculated. Photoluminescence study shows that the grown crystal is free from major defects. Crystalline perfection of the grown crystal was assessed and found good. Ground state optimized geometry has been obtained by using DFT with 6-31G(d,p) basis set. HOMO and LUMO energy gap was found to be 6.01 eV and dipole moment was 1.65 D.     

Temperature self-compensation fiber-optic pressure sensor based on fiber Bragg grating and Fabry–Perot interference multiplexing

A high performance multiplexed fiber-optic sensor consisted of diaphragm-based extrinsic Fabry–Perot interferometer (DEFPI) and fiber Bragg grating (FBG) is proposed. The novel structure DEFPI fabricated with laser heating fusion technique possesses high sensitivity with 5.35 nm/kPa (36.89 nm/psi) and exhibits ultra-low temperature dependence with 0.015 nm/°C. But the ultra-low temperature dependence still results in small pressure measurement error of the DEFPI (0.0028 kPa/°C). The designed stainless epoxy-free packaging structure guarantees the FBG to be only sensitive to temperature. The temperature information is created to calibrate the DEFPI's pressure measurement error induced by the temperature dependence, realizing effectively temperature self-compensation of the multiplexed sensor. The sensitivity of the FBG is 10.5 pm/°C. In addition, the multiplexed sensor is also very easy to realize the pressure and the temperature high-precise high-sensitive simultaneous measurement at single point in many harsh environmental areas.     

Fabry–Pérot cavities based on chemical etching for high temperature and strain measurement

In this paper, two hybrid multimode/single mode fiber Fabry–Pérot (FP) cavities were compared. The cavities fabricated by chemical etching are presented as high temperature and strain sensors. In order to produce this FP cavity a single mode fiber was spliced to a graded index multimode fiber with 62.5 μm core diameter. The Fabry–Pérot cavities were tested as a high temperature sensor in the range between room temperature and 700 °C and as strain sensors. A reversible shift of the interferometric peaks with temperature allowed to estimate a sensitivity of 0.75 ± 0.03 pm/°C and 0.98 ± 0.04 pm/°C for the sensor A and B respectively. For strain measurement sensor A demonstrated a sensitivity of 1.85 ± 0.07 pm/μ? and sensor B showed a sensitivity of 3.14 ± 0.05 pm/μ?. The sensors demonstrated the feasibility of low cost fiber optic sensors for high temperature and strain.     

Multispectral pyrometry for surface temperature measurement of oxidized Zircaloy claddings

Non-contact temperature measurement in a nuclear reactor is still a huge challenge because of the numerous constraints to consider, such as the high temperature, the steam atmosphere, and irradiation. A device is currently developed at CEA to study the nuclear fuel claddings behavior during a Loss-of-Coolant Accident. As a first step of development, we designed and tested an optical pyrometry procedure to measure the surface temperature of nuclear fuel claddings without any contact, under air, in the temperature range 700–850 °C. The temperature of Zircaloy-4 cladding samples was retrieved at various temperature levels. We used Multispectral Radiation Thermometry with the hypothesis of a constant emissivity profile in the spectral ranges 1–1.3 µm and 1.45–1.6 µm. To allow for comparisons, a reference temperature was provided by a thermocouple welded on the cladding surface. Because of thermal losses induced by the presence of the thermocouple, a heat transfer simulation was also performed to estimate the bias. We found a good agreement between the pyrometry measurement and the temperature reference, validating the constant emissivity profile hypothesis used in the MRT estimation. The expanded measurement uncertainty (k = 2) of the temperature obtained by the pyrometry method was ±4 °C, for temperatures between 700 and 850 °C. Emissivity values, between 0.86 and 0.91 were obtained.     

Optical fiber strain and temperature sensor based on an in-line Mach–Zehnder interferometer using thin-core fiber

We propose and demonstrate a fiber in-line Mach–Zehnder interferometer using thin-core fibers. This in-line interferometer is composed of a short section of thin-core fiber inserted between two single mode fibers (SMF), and demonstrated as a strain and temperature sensor in this study. A strain sensitivity of ?1.83 pm/με with a measurement range of 0?2000 με, and the temperature sensitivity of ?72.89 pm/°C with a temperature variation of 50 °C are achieved. We also discussed that the influence of strain and temperature change on the relative power ratios among the excited cladding modes in thin-core fibers.     

Synthesis,growth and characterization of a semiorganic nonlinear optical single crystal: L-Valine cadmium bromide

A semiorganic nonlinear optical material L-valine cadmium bromide was synthesized and single crystal grown from an aqueous solution by the method of slow evaporation technique at room temperature. The grown crystal was characterized by Powder X-ray diffraction and FT IR studies. The LVCB crystallizes in monoclinic system with cell parameters a = 10.144(2) Å, b = 5.54(1) Å, c = 12.07(2) Å, β = 109.115(2)° with space group P₂₁. Thermal behavior and stability of crystal were studied using thermogravimetric analyses (TGA) and differential thermal analysis (DTA) techniques. The suitability of this material for NLO application was studied by optical absorption studies and second harmonic generation (SHG) efficiency measurement by Kurtz–Perry powder method.     

Thermographic diagnosis system and imaging algorithm by distributed thermal data using single infrared sensor

An infrared diagnosis device provides two-dimensional images and patient-oriented results that can be easily understood by the inspection target by using infrared cameras. However, this device has disadvantages such as large size, high price, and inconvenient maintenance. In this regard, this study has proposed a small diagnosis device for body heat using a single infrared sensor and implementing an infrared detection system using a single infrared sensor and an algorithm that represents thermography using the obtained data on the temperature of the point source. The developed system had a temperature resolution of 0.1 °C and reproducibility of ±0.1 °C. The accuracy was 90.39% at the error bound of ±0 °C and 99.98% at that of ±0.1 °C. To evaluate the proposed algorithm and system, the infrared images of the camera method were compared. To verify the device’s clinical applicability, thermal images with clinical meaning were obtained from a patient who had lesions.     

Kinetic study of isothermal crystallization process of Gd2Ti2O7 precursor's powder prepared through the Pechini synthetic approach

Crystallization process of Gd₂Ti₂O₇ precursor's powder prepared by Pechini-type polymerized complex route has been studied under isothermal experimental conditions in an air atmosphere. It was found that the crystallization proceeds through two-parameter Šesták–Berggren (SB) autocatalytic model, in the operating temperature range of 550 °C≤T≤750 °C. Based on the behavior of SB parameters (M, N), it was found that in the lower operating temperature range, the crystallites with relatively low compactness exist, which probably disclosed low dimensionality of crystal growth from numerous nucleation sites, where the amorphous solid is produced. In the higher operating temperature region (above 750 °C), it was established that a morphological well-defined and high-dimensional particles of the formed pyrochlore phase can be expected. It was found that at T=850 °C, there is a change in the rate-determining reaction step, from autocatalytic into the contracting volume mechanism.     

Effect of reaction temperature on the size and morphology of scorodite synthesized using ultrasound irradiation

Synthesis of scorodite (FeAsO₄·2H₂O) using dynamic action agglomeration and the oxidation effect from ultrasound irradiation was investigated. The effect of different reaction temperatures (90, 70, 50, and 30 °C) on the size and morphology of scorodite particles synthesized under O₂ gas flow and ultrasound irradiation was explored because the generation of fine bubbles depends on the solution temperature. At 90 °C, the size of scorodite particles was non-homogeneous (from fine particles (<1 μm) to large particles (>10 μm)). The oxidation–reduction potential (ORP) and yield at 90 °C showed lower values than those at 70 °C. The scorodite particles, including fine and non-homogeneous particles, were generated by a decrease in the oxidation of Fe(II) to Fe(III) and promotion of dissolution caused by the generation of radicals and jet flow from ultrasound irradiation. Using ultrasound irradiation in the synthesis of scorodite at low temperature (30 °C) resulted in the appearance of scorodite peaks in the X-ray diffraction (XRD) pattern after a reaction time of 3 h. The peaks became more intense with a reaction temperature of 50 °C and crystalline scorodite was obtained. Therefore, ultrasound irradiation can enable the synthesis of scorodite at 30 °C as well as the synthesis of large particles (>10 μm) at higher temperature. Oxide radicals and jet flow generated by ultrasound irradiation contributed significantly to the synthesis and crystal growth of scorodite.     

Characterization of Young’s modulus of silicon versus temperature using a “beam deflection” method with a four-point bending fixture

Young’s modulus (E) and Poisson’s ratio (ν) are dependent upon the direction on the silicon surface. In this work, E and ν of silicon have been calculated analytically for any crystallographic direction of silicon by using compliance coefficients (s₁₁, s₁₂, and s₄₄), and the values of E are confirmed experimentally by using a “beam deflection” method with a four-point bending fixture. Experimental results for E as a function of temperature from −150 °C to +150 °C are presented for (0 0 1) and (1 1 1) silicon wafers.     

Physical,electrochemical and supercapacitive properties of activated carbon pellets from pre-carbonized rubber wood sawdust by CO2 activation

The physical and electrochemical properties of the activated carbon pellet electrodes have been investigated. Activated carbon pellets were prepared from single step carbonization process of pre-carbonized rubber wood sawdust at a temperature of 800 °C that followed with a CO₂ activation process at temperature in the range of 700–1000 °C. The BET characterization on the sample found that the surface area of the carbon pellet increased with the increasing of the activation temperature. The optimum value was as high as 683.63 m² g⁻¹. The electrical conductivity was also found to increase linearly with the increasing of the activation temperature, namely from 0.0075 S cm⁻¹ to 0.0687 S cm⁻¹ for the activation temperature in the range of 700–1000 °C. The cyclic voltammetry characterization of the samples in aqueous solution of 1 M H₂SO₄ also found that the specific capacitance increased with the increasing of the activation temperature. Typical optimum value was shown by the sample activated at 900 °C with the specific capacitance was as high as 33.74 F g⁻¹ (scan rate 1 mV s⁻¹). The retained ratio was as high as 32.72%. The activated carbon pellet prepared from the rubber wood sawdust may found used in supercapacitor applications.     

Simultaneous measurement of refractive index and temperature using thinned fiber based Mach–Zehnder interferometer

A novel method for simultaneous measurement of refractive index and temperature based on a small core and cladding diameters thinned fiber Mach–Zehnder interferometer (MZI) using singlemode-multimode-thinned-multimode-singlemode (SMTMS) fiber structure is proposed. Experiments indicate that the selected two interference orders have sensitivities of ?16.1936 nm/RIU and 0.0534 nm/°C, and ?23.0473 nm/RIU and 0.0575 nm/°C, respectively, among RI range from 1.3325–1.3720 and temperature range from 22 °C–82 °C. We can thus use the coefficient matrix of these two peaks to simultaneously determine the surrounding refractive index and temperature. The fabrication is easy, safe and cost effective, includes only the fusion splicing, making the device properly attractive for practical sensor applications.     

Thermoluminescence response in gamma and UV irradiated Dy2O3 nanophosphor

Low temperature solution combustion method was employed to synthesize Dy₂O₃ nanophosphors using two different fuels (sugar and oxalyl dihydrazine (ODH)). Powder X-ray diffraction confirm pure cubic phase and the estimated particle size from Scherrer's method in sugar and ODH fuel was found to be 26 and 78 nm, respectively, and are in close agreement with those obtained using TEM and W–H plot analysis. SEM micrographs reveal porous, irregular shaped particles with large agglomeration in both the fuels. An optical band gap of 5.24 eV and 5.46 eV was observed for Dy₂O₃ for sugar and ODH fuels, respectively. The blueshift observed in sugar fuel is attributed to the particles size effect. Thermoluminescence (TL) response of cubic Dy₂O₃ nanophosphors prepared by both fuels was examined using gamma and UV radiations. The thermoluminescence of sugar used samples shows a single glow peak at 377 °C for 1–4 kGy gamma irradiations. When dose is increased to 5 kGy, two more shouldered peaks were observed at 245 and 310 °C. However, in TL of ODH used samples, a single glow peak at 376 °C was observed. It is observed that TL intensity is found to be more in sugar used samples. In UV irradiated samples a single glow peak at 365 °C was recorded in both the fuels with a little variation in TL intensity. The trapping parameters were estimated by different methods and the results are discussed.     

Large-range liquid level sensor based on an optical fibre extrinsic Fabry–Perot interferometer

We propose an efficient approach to develop large-range liquid level sensors based on an extrinsic Fabry–Perot optical fibre interferometer with an all fused-silica structure and CO₂ laser heating fusion bonding technology. The sensor exhibits signatures of a high sensitivity of 5.3 nm/kPa (36.6 nm/psi), a resolution of 6.8 Pa (9.9×10⁻⁴ psi) and an extreme low temperature dependence of 0.013 nm/°C. As a result, a high resolution of the water level measurement of approximately 0.7 mm on the length scale of 5 m and small errors of the water pressure measurement induced by the temperature dependence within 0.0025 kPa/°C (0.00036 psi/°C, water level 0.25 mm/°C) are achieved, thus providing useful applications for the detection of the large-range liquid level in harsh environments.     

Preparation of cadmium stannate films by spray pyrolysis technique

Cadmium stannate thin films were prepared by spray pyrolysis technique using cadmium acetate and tin(II) chloride precursors at substrate temperatures 450 °C and 500 °C. XRD pattern confirms the formation of orthorhombic (1 1 1) cadmium stannate phase for the film prepared at substrate temperature of 500 °C, whereas, films prepared at 450 °C are amorphous. Film formation does not occur at substrate temperature from 300 to 375 °C. SEM images reveal that the surface of the prepared Cd₂SnO₄ film is smooth. The average optical transmittance of ∼86% is obtained for the film prepared at substrate temperature of 500 °C with the film thickness of 400 nm. The optical band gap value of the films varies from 2.7 to 2.94 eV. The film prepared at 500 °C shows a minimum resistivity of 35.6 × 10⁻⁴ Ω cm.     

Regenerated fibre Bragg grating fabricated on high germanium concentration photosensitive fibre for sensing at high temperature

A Regenerated Fibre Bragg Grating (RFBG), with repeatable high temperature response between 400 °C–1200 °C, has been demonstrated using a hydrogen-loaded, highly germanium-doped, photosensitive fibre. A wavelength shifts of as much as 20 nm is attained during temperature calibration up to 1300 °C. A large temperature response of 17 pm/°C is obtained from the RFBG, with very good repeatability.     

Characterization of Laves phase in Crofer 22 H stainless steel

This study investigated the effect of annealing temperature on the precipitation behavior of Crofer^® 22 H at 600 °C, 700 °C, and 800 °C. The grain size distribution, precipitate phase identification, and microstructure were analyzed using electron backscatter diffraction (EBSD) and energy dispersive X-ray spectroscopy (EDS). The morphology of Laves phase (Fe,Cr,Si)₂(Nb,W) precipitates having the Cr₂Nb structure changed from strip-like to needle-shaped as the annealing temperature was increased. The precipitates of the Laves phase also shifted from the grain boundaries to the grain interiors when the temperature was increased. However, the average grain size (150 μm) of the ferritic matrix did not significantly change at 600 °C, 700 °C, and 800 °C for 10 h.     

Densification and microstructure of lead zirconate titanate ceramics fabricated from a triol sol–gel powder

Lead zirconate titanate (PZT) nano-powder was prepared by a triol sol–gel process. X-ray diffraction and transmission electron microscopy results showed that as-synthesized amorphous powder started to crystallize at the calcination temperature above 500 °C. The crystalline powder was formed into pellets and sintered at temperatures between 900 and 1300 °C. Co-existence of tetragonal and rhombohedral phase was observed in all ceramics. Microstructural investigation of PZT ceramics showed that uniform grain size distribution with average grain size of ∼0.8–2.5 μm were received with sintering temperature up to 1200 °C. Further increasing the temperature caused abnormal grain growth with the grain as large as 13.5 μm. An attempt to optimize densification with uniform grain size distribution was also performed by varying heating rate and holding time during sintering. It was found that dense (∼97%) sol–gel derived PZT ceramic with uniform microstructure was achieved at 1100 °C with a heating rate of 5 °C min⁻¹ and 6 h dwell time.     

Effect of ultrasound energy on the zeolitization of chemical extracts from fused coal fly ash

This paper investigates the effects of ultrasound (UTS) energy at different temperatures on the zeolitization of aluminosilicate constituents of coal fly ash. UTS energy irradiated directly into the reaction mixture utilizing a probe immersed into the reaction mixture, unlike previously reported works that have used UTS baths. Controlled synthesis was also conducted at constant stirring and at the same temperatures using conventional heating. The precursor reaction solution was obtained by first fusing the coal fly ash with sodium hydroxide at 550 °C followed by dissolution in water and filtration. The synthesized samples were characterized by XRF, XRD, SEM and TGA. The crystallinity of crystals produced with UTS assisted conversion compared to conventional conversion at 85 °C was twice as high. UTS energy also reduced the induction time from 60 min to 40 min and from 80 min to 60 min for reaction temperatures of 95 °C and 85 °C, respectively. Prolonging the UTS irradiation at 95 °C resulted in the conversion of zeolite-A crystals to hydroxysodalite, which is a more stable zeolitic phase. It was found that at 85 °C coupled with ultrasound energy produced the best crystalline structure with a pure single phase of zeolite-A. It has been shown that crystallization using UTS energy can produce zeolitic crystals at lower temperatures and within 1 h, dramatically cutting the synthesis time of zeolite.     

Optically stimulated luminescence from BeO ceramics: An LM-OSL study

Optically Stimulated Luminescence (OSL) signals of BeO ceramics were investigated using continuous wave (CW) OSL and Linearly Modulated (LM) OSL. It was found that both curves can be approximated using a linear combination of two first-order components. Experiments on the measurement temperature dependence have shown that these two components have nearly the same thermal quenching energies around 0.57 eV. Dependences of the OSL signal on preheat temperature and radiation dose were also examined. Thermal annealing experiments have shown that OSL signals originate from traps which are unstable near 340 °C, thus proving the suitability of the signals for dosimetric purposes. Dose response was found to be linear and a minimum detectable dose of ～10 μGy was found.