Etchability of Latent Fission Fragment Tracks in CR-39

We report the chemical etching behaviour of the CR-39 polymer detector exposed to fission fragments of 252Cf describing etchability of latent tracks, which are like nanocylinders. The fission fragment exposed detectors were etched in 1-7 N NaOH water solutions at temperatures 50-80℃ for 45 min in the case of track length and 180 min in the case of track diameter measurements. The reduced etch rate S （called here etchability） is determined using experimental results for all etching conditions and the etching conditions with the highest reduced etch are obtained. Physics and energetics of bulk and track etching are discussed. Possible effects causing spurious changes in determination of activation energy of etching are investigated.     

Track revelation and optical properties of pentaerythritol tetrakis (allyl carbonate) plastic for application as nuclear track detector: effects of gamma radiations

The etching conditions of an indigenously prepared thin film of pentaerythritol tetrakis(allyl carbonate) (PETAC) were standardised for the use as a nuclear track detector. The optimum etching times in 6?N NaOH at 70°C for the appearance of fission and alpha tracks recorded in this detector from a ²⁵²Cf solid source were found to be 30 min and 1.50?h, respectively. The experimentally determined values for the bulk and track-etch rates for this detector in 6?N NaOH at 70°C were found to be 1.7?±?0.1 and 88.4?±?10.7?µm/h, respectively. From these results, the important track etching properties such as the critical angle of etching, the sensitivity and the fission track registration efficiency were calculated and compared with the commercially available detectors. The activation energy value for bulk etching calculated by applying Arrhenius equation to the bulk etch rates of the detector determined at different etching temperatures was found to be 0.86?±?0.02?eV. This compares very well with the value of about 1.0?eV reported for most commonly used track detectors. The effects of gamma irradiation on this new detector in the dose range of 200–1000?kGy have also been studied using bulk etch rate technique. The activation energy values for bulk etching calculated from bulk etch rates measurements at different temperatures were found to decrease with the increase in gamma dose indicating scission of the detector due to gamma irradiation. The optical band gap of this detector was also determined using UV–visible spectrometry and the value was found to be 4.37?±?0.05?eV.     

Results of high temperature processing of high-carbon materials from the lower Cambrian period of the Earth’s history

The paper reports on the observation of spontaneous fission of nuclides, concentrated in fly ash during the combustion of high-carbon (graphite) material, chemogenic siliceous-carbonaceous rocks and carbonaceous shale in the mixture with brown coal. In the samples obtained, the spontaneous fission was measured by track method. The zones of precipitation of spontaneous fission of nuclides and their lighter homologues on thermochromatographic column were determined. A nuclide with a half-life of 62 days was detected in the alkaline trap. The chemical treatment procedure included co-precipitation with iron hydroxide, dissolution in NH₄OH + H₂O₂ solution and distillation by heating up to 100°C followed by AgI co-precipitation. Based on the chemical behavior it can be concluded that the detected radionuclide belongs to the halides. The content of the parent nuclide in high-carbon (graphite) material and chemogenic siliceous-carbonaceous rock corresponds to 10^–14 g/g.     

Effect of annealing temperature on optical and electrochemical properties of chitosan–ZnO nanostructure

Chitosan–ZnO nanostructures were prepared by chemical precipitation method using different concentration of zinc chloride and sodium hydroxide solutions. Nanorod-shaped grains with hexagonal structure for samples annealed at 300 °C and porous structure with amorphous morphology for samples annealed at 600 °C were revealed in SEM analysis. X-ray diffraction patterns confirmed the hexagonal phase ZnO with crystallite size found to be in the range of ~24.15–34.83 nm. Blue shift of UV–Vis absorption shows formation of nanocrystals/nanorods of ZnO with marginal increase in band gap. Photoluminescence spectra show that blue–green emission band at 380–580 nm. The chitosan–ZnO nanostructures used on surface of a glassy carbon electrode gives the oxidation peak potential at ~0.6 V. The electrical conductivity of chitosan–ZnO composites were observed at 2.1?×?10^?5 to 2.85?×?10^?5?S/m. The nanorods with high surface area and nontoxicity nature of chitosan–ZnO nanostructures observed in samples annealed at 300 °C were suitable as a potential material for biosensing.     

Dissolution patterns caused by chemical etching of Al–Co–Cu and Al–Co–Ni decagonal quasicrystals with a HF–HNO3–H2O solution

Dissolution patterns essential for Al–Co–Cu and Al–Co–Ni decagonal quasicrystals (d-QCs) have been investigated in detail by chemical etching using a HF–HNO₃–H₂O solution followed by scanning electron microscopy (SEM) observations. The chemical etching of definite surface areas of the samples, which are either normal or parallel to the tenfold axes, using a solution with HF–HNO₃–H₂O (1?:?5?:?4 in volume ratio; 0°C; 5–10?min), produces a large number of microfacet pits of decagonal prismatic shape. In addition, the same etching test in combination with SEM observations was carried out on a deformed sample of the Al–Co–Ni d-QC, which had been subjected to concentrated mechanical stress at an elevated temperature of 850°C by means of the Vickers indentation technique. The morphological features of the resulting micropits and their possible origins are discussed on the basis of results obtained by SEM observations.     

Synthesis and properties of polyvinylidene fluoride high-temperature treatment products

Simultaneous thermal, gravimetric and mass spectrometric analyses made it possible to reveal considerable differences in fluorine desorption and changes in weight of filmy samples of original and partly chemically dehydrofluorinated polyvinylidene fluoride (PVDF) under an increase in temperature up to 800°C in argon flow. To determine the thermal treatment effect on the final material’s properties, the PVDF film was heated in a backing vacuum (0.5 Torr) up to 600°C with 40-minute isothermal exposure at a maximum temperature. Raman scattering spectroscopy was applied to compare molecular structures of the final products obtained by the high-temperature treatment of all samples and to prove their similarity. The spectrum of the chemically dehydrofluorinated sample, not subjected to a thermal effect, was characterized by a weak band in the region of 2000–2200 cm^–1, characteristic of the carbyne-like structures dominated by a polyyne type.

     

Influence of neutron irradiation on etching of SiC in KOH

The effect of reactor neutron irradiation on the etch rate of SiC in potassium hydroxide has been studied. In the case of high irradiation doses (10¹⁹–10²¹ cm^–2), the etch rate of silicon carbide has been shown to drastically rise, especially in the [0001]Si direction. This considerably mitigates the orientation anisotropy of polar face etching. After high-temperature annealing (up to 1200–1400°C), a higher etch rate of irradiated crystals persists. The results have been explained by the high concentration of radiation-induced (partially clustered) defects they contain.

     

Electrocaloric response in a relaxor ferroelectric polymer at temperatures far below the dielectric maximum

ABSTRACT

Relaxor ferroelectric polymer poly(vinylidene fluoride–trifluoroethylene–chlorofluoroethylene) (P(VDF-TrFE-CFE)) and its blends have been shown to exhibit a giant electrocaloric effect (ECE) over a broad temperature range, e.g. from 0 to 50 °C. Here, a special calorimeter was designed to directly characterize the heat absorbed Q_ECE due to ECE cooling of the blend of P(VDF-TrFE-CFE) with P(VDF-TrFE) 65/35 mol% copolymer down to ?15 °C, which covers the temperature range for many refrigeration applications. From Q_ECE, the isothermal entropy change ΔS and adiabatic temperature change ΔT are deduced. The data reveal that at ?15 °C the relaxor terpolymer/copolymer blend generates ΔS = 23.0J kg^?1 K^?1 and ΔT = 5.1K under 100 MV/m, which are still more than 65% of the ECE at room temperature. This temperature is far below the dielectric peak temperature of the relaxor blend and the results reveal the promise of the relaxor polymers for a broad range of EC cooling applications.     

An isothermal titration calorimetry study of the interactions between an oxyphenylethylene/oxyethylene diblock copolymer and sodium dodecyl sulfate

Interactions between the diblock copolymer S₁₅E₆₃ and the surfactant sodium dodecyl sulfate (SDS) have been investigated by isothermal titration calorimetry (ITC) in the temperature range 10–40°C. At 20°C, the block copolymer is associated into micelles with a hydrodynamic radius of 11.6?nm, which is composed of a hydrophobic styrene oxide (S) core and a water-swollen oxypolyethylene (PEO) corona. The copolymer/surfactant system has been studied at a constant copolymer concentration of 0.25?wt% and over a wide range of surfactant concentration, from 7.5?×?10^?6 up to 0.3?M. The titration calorimetric data for SDS in the temperature range 10–20°C presents a first endothermic increase indicating the formation of mixed copolymer rich-surfactant micelles. From that point, important differences in the ITC plots for surfactant titrations in the presence and in the absence of the copolymer are present. A shallow second endothermic peak is assigned to the interaction between SDS molecules and copolymer molecules resulting from the beginning of micelle disruption. An exothermic peak indicates the end of this disruption where only SDS micelles attached to single copolymer monomers are present, as shown by DLS in a previous paper. At higher temperatures in the range 25–40°C, the first endothermic maximum is not totally shown because interactions between surfactant and block copolymer start at very low SDS concentrations. Moreover, the second endothermic peak is absent and the exothermic minimum is less pronounced as a consequence of the increased micellization of the block copolymer.     

The thermal decomposition of mono-, di-, and tripotassium salts of trinitrophloroglucinol

The kinetics of the thermal decomposition of mono-, di-, and tripotassium salts of trinitrophloroglucinol (TNPG) was studied in the solid phase by the manometric method at m/V from 1 × 10^?4 to 15 × 10^?4 g/cm³ over the temperature ranges 125–150°C (K₁TNPG), 200–230°C (K₂ TNPG), and 200–250°C (K₃ TNPG). All the compounds decomposed according to the topochemical mechanism: there was an induction period, after which the rate of gas release was maximum. This rate then gradually decreased. The second decomposition stage was observed for K₁TNPG as the temperature increased to 200–250°C. The special features of changes in the rate of the process during transformation and the influence of the degree of vessel filling with a substance, particle size, and temperature on the kinetics of decomposition were studied. The kinetic results and composition of gaseous products and some condensed decomposition products lead to certain conclusions concerning the mechanism of the chemical transformations.     

Optical transmittance and microgravimetric studies of the oxidation of 〈100〉 single crystal films of copper

Thin single crystal copper films have been grown and oxidized on (100) faces of cleaved sodium chloride discs suspended from a vacuum ultramicrobalance. Optical transmittance measurements between 400–800 nm and electron microscopic investigations were also used to characterize the oxidation process. Polycrystalline copper films grown at room temperature are substantially the same as those grown previously on glass substrates. Single crystalline growth at 325 ° C on rock salt produces a characteristic transmittance curve due to the “island” nature of the films. These curves compare favorably with other previously published results. Single crystal copper films oxidized to CuO_0.67 at temperatures of 117–159°C in 100 Torr of oxygen for films less than 500 A thick. For films 378 to 1000 Å thick, compositions of CuO_0.52 to CuO_0.62 were obtained between 123–176°C. The oxidation to less than CuO_0.67 is attributed to the existence of islands in these films which are thicker than the average film thickness, and require higher temperatures or thinner films to permit oxidation to CuO_0.67 before the nucleation of CuO sets in.     

Operation of PEFC using composite sheets composed of phosphosilicate gels and thermally stable organic polymers

Thermally stable, flexible, and proton conductive composite sheets have been prepared from phosphosilicate (P₂O₅–SiO₂, P/Si = 1 in mole ratio) gel powder and several kinds of organic polymers. The organic polymers examined were polyimide (PI), polyamideimide (PAI), polyvinylidene fluoride (PVdF) and styrene–ethylene–butylenes–styrene elastomer (SEBS). PI and PAI effectively improved the chemical durability of the composite sheets by depressing the leaching of phosphoric acid from the gel. PVdF and SEBS provided the composite sheets with an excellent flexibility. Fuel cells using the membrane electrode assembly (MEA) composed of the composite sheet as an electrolyte and Pt-loaded carbon paper sheets as electrodes operated at temperatures in the range from room temperature to medium temperatures (∼ 150 °C).     

Extraction of tungsten from scheelite using hydrodynamic and acoustic cavitation

The primary purpose of this study is to investigate the effects of hydrodynamic and acoustic cavitation (HAC) on the leaching efficiency of tungsten. The aim is to reduce energy use and to improve the recovery rate. The goal is also to carry out a leaching process at a much lower temperature than in an autoclave process that is currently used in the industry. Energy-efficient initiation and collapse of cavitation bubbles require optimization of (i) vibro-acoustic response of the reactor structure, (ii) multiple excitation frequencies adapted to the optimized reactor geometry, and (iii) hydrodynamic cavitation with respect to orifice geometry and flow conditions. The objective is to modify and apply a previously in house developed high power cavitation reactor in order to recover tungsten by leaching of the dissolution of scheelite in sodium hydroxide. In this process, various experimental conditions like dual-frequency excitation, different orifice geometry have been investigated. The numerically optimized reactor concept was excited by two frequencies 23 kHz and 39–43 kHz in various flow conditions. The effects of leaching time, leaching temperature, ultrasonic power and geometry of orifice plates have been studied. The leaching temperature was varied from 40 °C to 80 °C. The concentration of leaching reagent sodium hydroxide (NaOH) was 10 mol/L.The results were compared to conventional chemical leaching. Energy supplement with acoustic cavitation of 130 kWh/kg concentrate resulted in a leaching recovery of tungsten (WO₃) of 71.5%, compared to 36.7% obtained in absence of ultrasound. The results confirm that the method developed is energy efficient and gives a recovery rate potentially better than current autoclave technology.     

Electrochemical properties of polyaniline-modified sodium vanadate nanomaterials

Sodium vanadate nanomaterials were synthesized at different pH-values of a sodium hydroxide solution of vanadium pentoxide. Polyaniline-modified sodium vanadate nanomaterials were prepared at room temperature and at 3°C by a chemical polymerization method. The crystal structure and phase purity of the samples have been examined by powder XRD. The samples were identified as HNaV₆O₁₆⋅4H₂O and Na_1.1V₃O_7.9. The electrochemical measurements show that polyaniline-modified sodium vanadate hydrated nanomaterials provide higher current density than the sodium vanadate nanomaterials.     

Crystallization behaviour in a new multicomponent Ti16.6Zr16.6Hf16.6Ni20Cu20Al10 metallic glass developed by the equiatomic substitution technique

A new amorphous Ti_16.6Zr_16.6Hf_16.6Ni₂₀Cu₂₀A1₁₀ alloy has been developed using the novel equiatomic substitution technique. Melt spinning Ti_16.6Zr_16.6Hf_16.6Ni₂₀Cu₂₀A1₁₀ forms an amorphous phase with a large supercooled liquid region, ΔT=70°C. After isothermal annealing within the supercooled liquid region for 3 h at 470°C, the amorphous alloy crystallizes to form a fine-scale distribution of 2–5 nm nanocrystals, and the supercooled liquid region increases to ΔT=108°C. Atomic-scale compositional analysis of this partially crystalline material using a three-dimensional atom probe (3DAP) is unable to detect any compositional difference between the nanocrystals and the remaining amorphous phase. After annealing for 1 hr at 620°C, the amorphous alloy crystallizes to form 20–50nm equiaxed grains of a hexagonal-type C14 Laves phase with lattice parameters a = 5.2Å and c = 9.0 Å. 3DAP analysis shows that this Laves phase has a composition very close to that of the initial amorphous phase, suggesting that the alloy crystallizes via a polymorphic rather than a primary crystallization mechanism, despite the complexity of the alloy composition.     

Diffusion and lattice location of lithium in zinc telluride

The diffusion of Li in ZnTe has been investigated in the temperature range 400–700°C by use of nuclear analysis and chemical or ion beam etching techniques. The penetration profiles are complex and most of them were found to show three regions. The experimental results are interpreted as a superposition of different diffusion mechanisms: one where the impurity diffuses simultaneously in substitutional and interstitial forms, the interstitial form being trapped at defects, and the other which involves short-circuit paths. Activation energies and diffusion constants D_o were measured. Furthermore the channeling technique was used for lattice location. This revealed that (60–80)% of the lithium atoms occupy the zinc substitutional site following annealing at 500°C.     

Fission cross section and fragment angular distribution in gold fission induced by 55 MeV alpha particles using solid state nuclear track detectors

The angular distribution of fission fragments in alpha induced fission has been studied at an incident energy of 55 MeV in¹⁹⁷Au target. The relative differential fission cross sections were measured at different angles between 10° and 170° and the resulting angular distributions fitted by least squares method with Legendre polynomials. In the present work, a correction for the self-scattering and self-absorption of fission fragments in the target itself was applied and a target of 3 mg/cm² was used to get good statistics. The anisotropy for 55 MeV alpha induced fission of gold was 2·83±0·43 and the fission cross section calculated by integrating the measured angular distributions over all the solid angles was 5·2±1.0 mb, confirming the value of 4·0±0·05 mb reported by Burnettet al but contrary to the high value of 10±3 mb reported by Ralarosyet al.     

Moderate hydrostatic pressure–temperature combinations for inactivation of Bacillus subtilis spores

We report the effect of using moderate hydrostatic pressure, 40–140?MPa, at moderate temperature (38–58°C) to inactivate Bacillus subtilis spores in McIlvaine's citric phosphate buffer at pH 6. We have investigated several parameters: pressure applied, holding time, pressure cycling, and temperature. The kinetics of spore inactivation is reported. The results show that spore inactivation is exponentially proportional to the time the sample is exposed to pressure. Spore germination and inactivation occur at the hydrostatic pressures/temperature combinations we explored. Cycling the pressure while keeping the total time at high pressure constant does not significantly increase spore inactivation. We show that temperature increases spore inactivation at two different rates; a slow rate below 33°C, and at a more rapid rate at higher temperatures. Increasing pressure leads to an increase in spore inactivation below 95?MPa; however, further increases in pressure give a similar rate kill. The time dependence of the effect of pressure is consistent with the first-order model (R²?>?0.9). The thermal resistance values (Z_T) of B. subtilis spores are 30°C, 37°C, and 40°C at 60, 80, 100?MPa. The increase in Z_T value at higher pressures indicates lower temperature sensitivity. The pressure resistance values (Z_P) are 125, 125 and 143?MPa at 38°C, 48°C, and 58°C. These Z_P values are lower than those reported for B. subtilis spores in the literature, which indicates higher sensitivity at pressures less than about 140?MPa. We show that at temperatures <60°C, B. subtilis spores are inactivated at pressures below 100?MPa. This finding could have implications for the design of the sterilization equipment.     

Size effect on the Mie optical absorption of small sodium particles in sodium azide NaN3

The Mie optical absorption spectra of colloidal sodium particles in sodium azide NaN₃ has been measured and compared with calculated spectra. The small particles were formed by X irradiating single crystals of the azide and then heating them at 280° C. The peak was observed to occur at about 5200 Å compared to the calculated position of 5020 Å. By comparing the measured and calculated spectra, the approximate particle size was deduced as a function of the heating time. For a given anneal time the size was found to be approximately independent of the irradiation dose, whilst the concentration of particles increased rapidly with increasing dose. After an anneal of 2 min the particle size was between 10 and 20 Å, increasing to about 100 Å after 12 min and about 1000 Å after 30 min.     

Reflectometric studies of the etching of a silica fiber with a germanium silicate core in sub- and supercritical water

Fiber optic reflectometry (FOR) and scanning electron microscopy (SEM) were used to study the regularities of the etching of a single-mode optical silica fiber with a germanium silicate core in subcritical and supercritical water. It was demonstrated that the rate of etching of the germanium silicate core, being higher than that of etching of the silica cladding, was responsible for the formation of a well at the fiber end face, the depth of which increased with the time of etching. The temporal behavior of the FOR signal was of oscillatory character, an observation that accounted for the interference effects that accompany the reflection of radiation (from the photodiode used in the FOR) from the fiber end face during its etching (well deepening). The interference-controlled character of the FOR signal made it possible to directly measure the rate of etching of the fiber end face in water in its different phase states (gaseous, liquid, and supercritical) at various temperatures and pressures. The lowest measured rate of etching of the germanium silicate core (at 200°C and 54 atm) was 10⁻³ nm/s, whereas the highest measured rate was 30 nm/s (at 400°C and 246 atm). The temperature dependence of the etching rate was demonstrated to obey the Arrhenius law, with an activation energy of 58 ± 3 kJ/mol. At later stages of etching, the FOR signal changed from regular oscillatory to irregular noisy due to the formation defects of various sizes, as could be clearly seen in SEM images.