Registration temperature effect on sensitivity of CR-39(DOP) and SR-90 polymer track detectors

The samples of CR-39(DOP) and SR-90 polymer track detectors have been exposed to -particles from ²⁴¹Am source in an exposure unit. The temperature of the detectors during irradiation has been varied from −30°C to 70°C. These exposed samples have been etched in 6.25 N NaOH solution at 60°C for various etching times. The variation of sensitivity of these detectors as a function of registration temperature has been studied. It has been observed that at the fixed registration temperature, the sensitivity of SR-90 is more than CR-39(DOP) polymer track detector. However, the enhancement in sensitivity with the decrease in registration temperature is more pronounced in case of CR-39(DOP) than SR-90.     

The effect of etching solution composition on the response of an electrochemically etched CR-39 detector

Etching solutions of different compositions were applied at room temperature (22°C) for electrochemical etching. The background developed during electrochemical etching in a CR-39 track detector was investigated. Detectors irradiated with alphas of 5.49 MeV were measured also. It was found that the PEW solutions (potassiumhydroxid, ethylalcohol, water) showed good sensitivity. One of them (PEW_20/40 was applied for neutrons from a ²⁵²Cf source. The achieved registration sensitivity was about 10⁻⁵ spot/n after 3 hours of etching time.     

Silver ionic conductivity enhancement by network former mixed in oxide-based glasses

Glasses in the binary system xAg₂P₂O₆ − (1 − x)Ag₂Te₂O₅ have been prepared for 0 x 1. For each composition only one glass transition temperature is observed in the temperature range of 180–220 °C. All glasses appear homogeneous considering their optical and electrical properties. Nevertheless, in SEM observations, some glass compositions appear to be heterogeneous after decoration following short nitric acid etching. For each composition, conductivity data obtained in the temperature range of 25–200 °C using impedance techniques obey an Arrhenius relationship with a composition independent pre-exponential term. Variation of the conductivity activation energy with x induces correlative variations of isothermal conductivity curves leading to an increase of the ionic conductivity of about one order of magnitude compared with linearity at 25 °C. This behaviour is discussed with respect to the thermodynamic properties of the glassy solutions.     

The influence of different fabrication processes on characteristics of excess Bi2O3-doped 0.95 (Na0.5Bi0.5)TiO3–0.05 BaTiO3 ceramics

In this study, we will develop the influences of the excess x wt% (x=0, 1, 2, and 3) Bi₂O₃-doped and the different fabricating process on the sintering and dielectric characteristics of 0.95 (Na_0.5Bi_0.5)TiO₃–0.05 BaTiO₃ ferroelectric ceramics with the aid of SEM and X-ray diffraction patterns, and dielectric–temperature curves. The 0.95 (Na_0.5Bi_0.5)TiO₃–0.05 BaTiO₃+x wt% Bi₂O₃ ceramics are fabricated by two different processes. The first process is that (Na_0.5Bi_0.5)TiO₃ composition is calcined at 850 °C and BaTiO₃ composition is calcined at 1100 °C, then the calcined (Na_0.5Bi_0.5)TiO₃ and BaTiO₃ powders are mixed in according to 0.95 (Na_0.5Bi_0.5)TiO₃–0.05 BaTiO₃+x wt% Bi₂O₃ compositions. The second process is that the raw materials are mixed in accordance to the 0.95 (Na_0.5Bi_0.5)TiO₃–0.05 BaTiO₃+x wt% Bi₂O₃ compositions and then calcining at 900 °C. The sintering process is carried out in air for 2 h from 1120 to 1240 °C. After sintering, the effects of process parameters on the dielectric characteristics will be developed by the dielectric–temperature curves. Dielectric–temperature properties are also investigated at the temperatures of 30–350 °C and at the frequencies of 10 kHz–1 MHz.     

Effect of branching in base polymer on ionic conductivity in hyperbranched polymer electrolytes

Novel hyperbranched polymer, poly[bis(diethylene glycol)benzoate] capped with a 3,5-bis[(3′,6′,9′-trioxodecyl)oxy]benzoyl group (poly-Bz1a), was prepared, and its polymer electrolyte with LiN(CF₃SO₂)₂, poly-Bz1a/LiN(CF₃SO₂)₂ electrolyte, was all evaluated in thermal properties, ionic conductivity, and electrochemical stability window. The poly-Bz1a/LiN(CF₃SO₂)₂ electrolyte exhibited higher ionic conductivity compared with a polymer electrolyte based on poly[bis(diethylene glycol)benzoate] capped with an acetyl group (poly-Ac1a), and the ionic conductivity of poly-Bz1a/LiN(CF₃SO₂)₂ electrolyte was to be 7×10⁻⁴ S cm⁻¹ at 80 °C and 1×10⁻⁶ S cm⁻¹ at 30 °C, respectively. The existence of a 3,5-bis[(3′,6′,9′-trioxodecyl)oxy]benzoyl group as a branching unit present at ends in the base polymer improved significantly ionic conductivity of the hyperbranched polymer electrolytes. The polymer electrolyte exhibited the electrochemical stability window of 4.2 V at 70 °C and was stable until 300 °C.     

Modifications in track registration response of PADC detector by energetic protons

It has been well established that different ionising radiations modify the track registration properties of dielectric solids. In an effort to study the response of Polyallyl diglycol carbonate (PADC Homalite) detector towards fission fragment, PADC detectors were exposed to 10⁴ Gy dose of 62 MeV protons and then one set of samples were exposed to fission fragments from a ²⁵²Cf source. Two of these detectors were containing a thin layer of Buckminsterfullerene (C₆₀). The study of the etched tracks by Leitz Optical Microscope reveals that the track diameters are enhanced by more than 70% in the proton irradiated zone as compared to that in the unirradiated zone. Scanning Electron Microscopy was performed after etching the sample in 6 N NaOH at 55°C for different etching times, to study the details of the surface modifications due to proton irradiation of PADC detectors with and without C₆₀ layer. Our observations revealed that the diameters and density of proton tracks have increased with etching time on the surface facing the fullerene layer as well as the other surface. However, a relatively more open structure of the etched surface containing C₆₀ as compared to the bare one may be an indication of the extra damage caused by the energy released upon the destruction of C₆₀ molecules by energetic protons.     

Hydrogen distribution in oxynitride/oxide structures

Silicon oxynitride films with five different O/N ratios were deposited with low pressure chemical vapor deposition on a silicon substrate covered with an oxide. The films were subjected to subsequent post-deposition anneals in N₂ and H₂ at 1000°C, and a H plasma at 300°C to obtain information about the hydrogen chemistry. The overall film compositions were determined with elastic recoil detection. The resonant reaction ¹⁵N(¹H, γ)¹²C was used to obtain hydrogen depth profiles. The hydrogen depth profiles are characterized by a value for the bulk concentration and width of the interfacial region. We found that the stability of the hydrogen in the bulk has a maximum for O/N ≈ 0.32. From the measured interfacial widths we deduced that for low values of O/N the stability of hydrogen in the interfacial region is relatively large. For intermediate values of O/N the stability of the hydrogen in the bulk and the interfacial region do not differ significantly, while for high O/N a relatively low stability of the interfacial hydrogen is observed. The O/N dependence of the stability of the interfacial hydrogen is consistent with the bulk stability if we assume that the interfacial oxynitride is oxygen enriched as compared to the bulk oxygen concentration.     

Polymer electrolytes based on ethylene oxide–epichlorohydrin copolymers

In this work we studied the ionic conductivity for three copolymers of the title co-monomers as a function of LiClO₄ content, temperature and ambient relative humidity. We also investigated the interactions between the salt and the co-monomer blocks in the copolymers and its effect on the morphology and thermal properties of the copolymer/salt complexes. Our data indicate that the Li⁺ ion predominantly interacts with the ethylene oxide repeating units of the copolymers. The copolymer with the highest ionic conductivity was obtained with an ethylene oxide/epichlorohydrin ratio of 84/16 containing 5.5% (w/w) of LiClO₄. It showed a conductivity of 4.1×10⁻⁵ S cm⁻¹ (30°C, humidity< 1 ppm) and 2.6×10⁻⁴ S cm⁻¹ at 84% relative humidity (24°C). The potential stability window of the copolymer/salt complex is 4.0 V, as measured by cyclic voltammetry. For comparison, we also prepared a blend of the corresponding homopolymers containing LiClO₄; it showed higher crystallinity and lower ionic conductivity.     

Structure and optical properties of sol–gel derived Gd2O3 waveguide films

Pure and rare earth doped gadolinium oxide (Gd₂O₃) waveguide films were prepared by a simple sol–gel process and dip-coating method. Gd₂O₃ was successfully synthesized by hydrolysis of gadolinium acetate. Thermogravimetric analysis (TGA) and differential thermal analysis (DTA) were used to study the thermal chemistry properties of dried gel. Structure of Gd₂O₃ films annealed at different temperature ranging from 400 to 750 °C were investigated by Fourier transform infrared (FT-IR) spectroscopy, X-ray diffraction (XRD) and transmission electron microscopy (TEM). The results show that Gd₂O₃ starts crystallizing at about 400 °C and the crystallite size increases with annealing temperature. Oriented growth of (4 0 0) face of Gd₂O₃ has been observed when the films were deposited on (1 0 0) Si substrate and annealed at 750 °C. The laser beam (λ=632.8 nm) was coupled into the film by a prism coupler and propagation loss of the film measured by scattering-detection method is about 2 dB/cm. Luminescence properties of europium ions doped films were measured and are discussed.     

Poly(ethylene oxide-co-epichlorohydrin)/NaI: a promising polymer electrolyte for photoelectrochemical cells

We have investigated the thermal and ionic conductivity properties of the elastomer poly(ethylene oxide-co-epichlorohydrin) filled with NaI and I₂. The reason for using this composition is its potential application as electrolyte in photoelectrochemical cells. This copolymer was characterized as a function of NaI concentration, temperature and relative humidity. According to the data obtained, the Na⁺ ion interacts with the ethylene oxide repeating units by means of Lewis type acid–base interactions. The empirical Vogel–Tamman–Fulcher equation was used to model the conductivity and temperature relationships, indicating that the conduction occurs in the amorphous phase of the copolymer. The sample with 9.0% (w/w) of NaI presents a conductivity of 1.5×10⁻⁵ S cm⁻¹ in a dry atmosphere (30°C, [H₂O]<1 ppm) and 2.0×10⁻⁴ S cm⁻¹ at 86% relative humidity (22°C).     

Barium ferrite particulates prepared by a salt-melt method

Barium ferrite particulates have been prepared by coprecipitation and calcination in a flux of NaCl-KCl. It was found that a flux containing more than 30 wt% KCl tends to seriously deteriorate the magnetic properties of resultant perticulates. The flux with 10 wt% KCl or less showed promising results. A Ba(CoZr)_0.75Fe_10.5O₁₉ particulate showed the best properties, i.e., a saturation magnetization of 68.5, a squareness ratio of 0.49, and a coercivity of 1280 Oe, when calcined in NaCl at 900°C for 4 h.     

Absorption and velocity dispersion due to crystallization and melting of emulsion droplets

The influence of droplet crystallization and melting on the ultrasonic properties of oil-in-water emulsions has been investigated. The ultrasonic velocity and attenuation were measured in a series of 3 wt% n-hexadecane-in-water emulsions as a function of frequency (0.3–4 MHz), droplet diameter (0.4 and 1 μm) and temperature (0–25°C). The emulsified n-hexadecane crystallized at about 5°C due to supercooling effects and melted at about 18°C. As solid and liquid n-hexadecane have significantly different ultrasonic properties, an appreciable change in the velocity and attenuation is observed during the phase transition. This behaviour is modified significantly in systems where the emulsion droplets are partially crystalline because the temperature fluctuations associated with the ultrasonic wave can perturb the phase equilibria solid liquid causing excess attenuation and velocity dispersion. The magnitude of this effect depends on the ultrasonic frequency and the average droplet size.     

Experimental study on the aging process of the LR 115 cellulose nitrate radon detector

An experimental determination of the aging process of cellulose nitrate detector material was based on the examination of special properties of the LR 115 solid state nuclear track detectors (SSNTDs) of various ages up to 18 years. The examined relevant parameters are the bulk etching rate v_b and the track etching rate v_t. These parameters are responsible for the appearance, the size and the registration efficiency of tracks of -particles from radon gas in the detector. To find a correlation between these material parameters and the detector sensitivity an experimental calibration of indoor room and outdoor soil detector devices based on LR 115 took place at the Umweltforschungszentrum Leipzig-Halle (Germany). To avoid routine calibration work in external radon exposure facilities a correction of the age dependent calibration factors with the material parameters measured in one's own laboratory was targeted. In this study a general age dependence, however, was not found. The following statements for practical applications can be made. (i) the bulk etching rate v_b for detectors of the same batch has a depth dependence and this dependence is constant over 2 years (LR 115 September 1994). (ii) detectors of different batches older than 5 years and stored at room temperature show an odd v_b behaviour when v_b is used for describing track shapes. (iii) the calibration factor of detectors of different batches that were stored at about +4°C is constant over 5 years (LR 115 September 1994 and February 1999, Table 2).

The conclusion is that LR 115 detectors not older than 5 years and stored in a refrigerator at about +4°C should be preferred for radon measurements. Furthermore these detectors should be recalibrated every year and the microscope work of this calibrations should be performed by the same person who performs the measurements.

In addition, a phenomenon related to fundamental track formation mechanisms was found, that the time straggling of the time t_through when vertical tracks penetrate the 12 μm thick detector layer is independent of the age of the detectors and the energy of the -particle at the detector surface.     

Comblike polymer electrolyte with main chain glass transition near room temperature

A new amorphous comblike polymer (CBP) based on methylvinyl ether/maleic anhydride altering copolymer backbone and on oligooxyethylene side chain was synthesized. The dynamic mechanical properties of CBP and its Li salt complexes were investigated by means of DDV-ll-EA type viscoelastic spectrometry. Results showed that there were two glass transitions (-transition and β-transition) in the temperature range from − 100 to 100 °C. The β-transition was assigned to oligo-PEO side chains and the temperature of β-transition increases with increasing Li salt content. The -transition was assigned to the main chain of CBP. The temperature of the -transition (T) is also dependent upon the Li-salt content, but not monotonie. The value of T lies between 30–45 °C in the Li salt concentration range studied, near room temperature. It was found that the CBP-Li salt complexes showed an unusual dependence of ionic conductivity on Li salt content. There are two peaks in the plot of the ionic conductivity vs. Li salt concentration, which has been ascribed to the movability of the CBP main chain at ambient temperature. The temperature dependence of the ionic conductivity indicated that the Arrhenius relationship was not obeyed, and the plot of log σ against 1/(T − T₀) showed the unusual dual VTF behavior when using side chain glass transition temperature (T_β) as T₀.     

Proton conductive amorphous thin films of tungsten oxide clusters with acidic ligands

Three kinds of peroxo-polytungstic acid (PPTA, C-PPTA and N-PPTA) were obtained by reacting hydrogen peroxide with metallic tungsten, tungsten carbide or tungsten nitride, respectively. Polytungstates, C-PPTA and N-PPTA, were found to contain oxalate and nitrate ligands. Their proton conductivities were compared using thin film specimens spin-coated from their water solution. Conductivity of each as-coated film was in the range from 10⁻³ to 10⁻⁴ S cm⁻¹ under the relative humidity of 40% (25 °C). A sharp decrease in conductivity (to less than 10⁻⁷ S cm⁻¹ at 25 °C) was observed for PPTA without acidic ligands after thermal treatment at 80 °C. However, the effect of thermal treatment on C-PPTA or N-PPTA was much milder. A 80 °C-treated C-PPTA film showed the conductivity of 1.0 × 10⁻⁵ S cm⁻¹ (25 °C) with a very weak dependency on ambient humidity.     

Electrical conducting properties of proton-conducting terbium-doped strontium cerate membrane

The electrical conduction behavior of SrCe_0.95Tb_0.05O_3−δ (SCTb) was investigated in different gases at high temperatures. In air, oxygen or nitrogen SCTb shows small electronic-hole conduction below 800°C and oxygen ionic conduction over 800°C with activation energy about 30 kJ/mol and 164–181 kJ/mol respectively. SCTb becomes a protonic conductor in hydrogen or methane in 500–900°C, with the proton conductivity in the range of 10⁻³–10⁻² S/cm, two to three orders of magnitude higher than electronic or oxygen ionic conductivity of SCTb in air or oxygen. The activation energy for protonic conduction in SCTb is 49 kJ/mol in methane and 54 kJ/mol in hydrogen. The electrical conductivity of SCTb in water vapor-saturated nitrogen, air or oxygen is higher than in corresponding gas without water vapor. Presence of water vapor does not affect the electrical conduction of SCTb in hydrogen or methane. Gas permeation measurements show that SCTb membrane is impermeable to hydrogen when the membrane is exposed to hydrogen or methane upstream and nitrogen or oxygen downstream. These results confirm that SCTb is a pure protonic conductor with very low electronic and oxygen ionic conductivity. SCTb will find applications as a high temperature electrolyte in fuel cells or hydrogen sensors.     

Transport properties of SrCe0.95Y0.05O3−δ and its application for hydrogen separation

Transport properties of SrCe_0.95Y_0.05O_3−δ were studied by impedance spectroscopy and by measuring open-cell voltage (OCV) and gas permeation. Ionic transference numbers were determined by measuring the OCV of concentration cells and water vapor evolution of an O₂/H₂ fuel cell. We observed interfacial polarization on the basis of the I–V curves obtained by discharging a hydrogen concentration cell or an O₂/H₂ fuel cell. The observed high protonic conductivity (high proton and low oxide ion transference numbers) makes SrCe_0.95Y_0.05O_3−δ a potential material for hydrogen separation. From proton conductivity measurements, under a given hydrogen partial pressure difference of 4%/0.488%, the hydrogen permeation rate (of a dense membrane with 0.11 cm in thickness) was calculated to be ≈0.072 cm³ (STP) cm⁻² min⁻¹ at 800°C, whereas the permeation rate calculated from short-circuit current measurements was ≈0.023 cm³ (STP) cm⁻² min⁻¹ at 800°C. The difference between calculated and observed permeation rates is probably due to interfacial polarization.     

Time evolution of interface roughness during thermal oxidation on Si(0 0 1)

The surface morphological change at an initial stage of thermal oxidation on Si(0 0 1) surface with O₂ was investigated as a function of oxide coverage by a real-time monitoring method of Auger electron spectroscopy (AES) combined with reflection high energy electron diffraction (RHEED). At 653 °C where oxide islands grow laterally, protrusions were observed to develop under the oxide islands as a consequence of concurrent etching of the surface. The rate of etching was measured from a periodic oscillation of RHEED half-order spot intensity I_(1/2,0) and I_(0,1/2). At 549 °C where Langmuir-type adsorption proceeds, it was observed that both I_(1/2,0) and I_(0,1/2) decrease more rapidly in comparison with an increase of oxide coverage and the intensity ratio between them decreases gradually with O₂ exposure time. These suggest that Langmuir-type adsorption occurs at sites where O₂ adsorbs randomly, leading to subdivision of the 2×1 and 1×2 domains by oxidized regions, and that Si atoms are ejected due to volume expansion in oxidation to change the ratio between 2×1 and 1×2 domains.     

Polymer electrolyte plasticized with PEG-borate ester having high ionic conductivity and thermal stability

We have focused on the PEG-borate ester as a new type of plasticizer for solid polymer electrolyte composed of poly(ethyleneglycol) methacrylate (PEGMA) and lithium bis-trifluoromethanesulfonimide (LiTFSI). The PEG-borate ester shows good thermal stability and high flash point. Ionic conductivity of the polymer electrolyte increases with increasing amount of the PEG-borate ester and exhibits values greater than 10⁻⁴ S cm⁻¹ at 30 °C and 10⁻³ S cm⁻¹ at 60 °C. Furthermore, PEG-borate ester has three EO chains whose lengths are variable, and various ionic conductivities are expected to depend on EO chain length. As a result, polymer electrolyte containing the PEG-borate ester whose EO chain length is n=3 shows highest ionic conductivity. Furthermore, polymer electrolytes containing PEG-borate esters show excellent thermal and electrochemical stability. The electrolytes are thermally stable up to 300 °C and electrochemically up to 4.5 V vs. Li⁺/Li.     

Magnetic hysteresis in rapidly quenched rare-earth alloys

The magnetic and structural properties of rapidly quenched (Pr₈₀Ga₂₀)_100-xFe_x, RTbFe and RTbFe(Co)M alloys are examined over a wide range of chemical compositions, where R ≡ Pr, Sm, MM and M ≡ B and Si. The Ga-containing samples show relatively high coercive fields (up to 3 kOe) in the amorphous state which subsequently disappear after crystallization. On the other hand, the high coercive fields (≈5 kOe) of melt-spun RTbFe samples decrease slightly after crystallization but their magnetic moment increases substantially. Melt-spun RTbFe(Co)M samples are generally magnetically soft in the as-quenched state. Magnetic hardening is produced by annealing the samples around 750°C leading to coercive fields which could not be measured with an ordinary electromagnet (H_c #62; 23 kOe). The best properties have been obtained on a Pr₁₄Fe₇₁B₁₅ sample with a coercive field of 8 kOe and an energy product of 8.5 MGOe. Thermomagnetic data show that a structural transformation takes place upon heating the samples to 750°C. The Curie temperature of the precipitate phase is around 320°C while that of the as-quenched phase is around 160°C. Transmission electron microscope studies show a very fine precipitate structure with a precipitate size below 100 Å. The precipitate phase is believed to be highly anisotropic leading to the observed hard magnetic properties.