A versatile integrated system for thermoluminescence and optically stimulated luminescence measurements

A versatile integrated reader system for TL and OSL measurements of phosphor materials has been described for luminescence research applications. The developed integrated reader system works either in TL or OSL or TL-OSL mode. In the OSL operation, besides the conventional CW-OSL, POSL and LM-OSL modes a novel non-linear OSL (NL-OSL) method has been incorporated in the reader system. The optical stimulation unit consists of four high power LEDs fitted in four channels and optically focused on the sample. Each of the LED is capable of delivering up to 80 mW/cm² light power at the sample position. The LEDs with peak wavelength λ_p ≈ 470 nm and 530 nm and Δλ ≈ 20 nm have been used for optical stimulation of the samples. A PID temperature controller has been used for generating and controlling user defined heating profiles for the TL measurements in the reader system. The reader system covers a wide dynamic dose range of 10 μGy to 10³ Gy for TL/OSL measurements. The OSL grade α-Al₂O₃:C phosphor was used to test the reader system and investigate its impact on low dose assessment for personnel and environmental monitoring. The design concept of the reader system and the results of dose measurements are discussed.     

Nanoparticles of Al2O3:Cr as a sensitive thermoluminescent material for high exposures of gamma rays irradiations

Aluminum Oxide (Al₂O₃) doped with proper activators is a highly sensitive phosphor commonly used for radiation dosimetry using thermoluminescence (TL) technique. Nanoparticles of this material activated with Chromium (Cr) have been synthesized using the propellant chemical combustion technique and studied for their TL response. They were characterized by X-ray diffraction and scanning electron microscope. The synthesized material has spherical nanoparticles with grain size around 25 nm. These nanoparticles were exposed to heavy doses from γ-rays of ¹³⁷Cs. The TL glow curves show a prominent peak at around 474 K. This peak is found to be sensitive for high exposures of γ-rays and has linear response in the range of 100 Gy-20 kGy without showing saturation. This remarkable result suggests that Al₂O₃:Cr nanoparticles might be used for the dosimetry of food and seed irradiations.     

Studies on new neutron-sensitive dosimeters using an optically stimulated luminescence technique

The neutron response of detectors prepared using α-Al₂O₃:C phosphor developed using a melt processing technique and mixed with neutron converters was studied in monoenergetic neutron fields. The detector pellets were arranged in two different pairs: α-Al₂O₃:C + ⁶LiF/α-Al₂O₃:C + ⁷LiF and α-Al₂O₃:C + high-density polyethylene/α-Al₂O₃:C + Teflon, for neutron dosimetry using albedo and recoil proton techniques. The optically stimulated luminescence response of the Al₂O₃:C + ^6,7LiF dosimeter to radiation from a ²⁵²Cf source was 0.21, in terms of personal dose equivalent H_p(10) and relative to radiation from a ¹³⁷Cs source. This was comparable to results obtained with similar detectors prepared using commercially available α-Al₂O₃:C phosphor. The H_p(10) response of the α-Al₂O₃:C + ^6,7LiF dosimeters was found to decrease by more than two orders of magnitude with increasing neutron energy, as expected for albedo dosimeters. The response of the α-Al₂O₃:C + high-density polyethylene/α-Al₂O₃:C + Teflon dosimeters was small, of the order of 1% to 2% in terms of Hp(10) and relative to radiation from a ¹³⁷Cs source, for neutron energies greater than 1 MeV.     

LiMgPO4:Tb,B OSL phosphor - CW and LM OSL studies

In the adjoining paper, the authors have proposed LiMgPO₄:Tb,B (LMP) OSL phosphor as a potential alternative to α-Al₂O₃:C for dosimetry applications. This calls for developing an understanding on TL and OSL aspects of this highly sensitive LMP phosphor. CW and LM OSL processes were therefore studied experimentally and kinetic analysis was carried out using theoretical models. Continuous wave (CW) OSL curve for LMP phosphor was found not to follow single decaying exponential implying that the CWOSL curve does not follow first order kinetics. Under pre-readout annealing at 125, 200 and 300 °C for 10 s, the nature of decay profile was unaffected and same holds true for optically bleached CWOSL curves. From linearly modulated (LM) OSL studies, it was found that the shape/geometrical factor μ_g was ∼0.72 ± 0.03 for wide range of doses (up to 12 Gy studied) and peak position “t_m” was also independent of dose. The μ_g was found to be unaffected with pre-readout annealing at 125, 200 and 300 °C for 10 s and optical bleaching, however it was found that peak position “t_m” shifted towards higher side in time with increase of optical bleaching. Dose dependence tests were also carried out for LMOSL curves and it was found that peak position “t_m” was independent of dose, which is typical characteristic of curves following first order kinetics. Hence LM-OSL curve might be mixture of more than one component.Further from CW and LM OSL studies, it was also found that the individual contribution from first, second and third TL peak toward OSL is ∼33%, ∼45% and ∼22%, respectively. Traps beyond 350 °C were found not to contribute towards OSL when stimulated using blue LEDs. In the present paper, the CW and LM OSL processes for LMP phosphor were studied experimentally and their kinetic analysis was carried out.     

Electronic sputtering of Gd3Ga5O12 and Y3Fe5O12 garnets: Yield, stoichiometry and comparison to track formation

The results of present paper have shown that sputtering of yttrium iron garnet (Y₃Fe₅O₁₂) under swift heavy ions in the electronic energy loss regime is non-stoichiometric. Here we are presenting additional experimental results for gadolinium gallium garnet (Gd₃Ga₅O₁₂) as target. The irradiations were performed with different ions (⁵⁰Cr (589 MeV), ⁸⁶Kr (195 MeV) and ¹⁸¹Ta (400 MeV)) impinging perpendicularly to the surface. As earlier, the sputtering yield was determined by collecting the emitted gadolinium and gallium atoms on a thin aluminium foil, placed upstream above the target and analyzing the Al catcher by Rutherford backscattering. Also for Gd₃Ga₅O_12, the emission of Gd and Ga is non-stoichiometric. Sputtering appears above a critical electronic stopping power of S_th = 11.6 ± 1.5 keV/nm, which is larger than the threshold for track formation, in agreement with other amorphisable materials. In addition, the angular distribution of the sputtered species was measured for Y₃Fe₅O₁₂ and Gd₃Ga₅O₁₂ using 200 MeV Au ions impinging the surface at 20° relatively to the surface. For the two garnets the ratio of Y/Fe (and Gd/Ga) varies with the angle of emitted species and the stoichiometry seems to be preserved only for an emission perpendicular to the surface.     

Depth profiling of Al2O3 + TiO2 nanolaminates by means of a time-of-flight energy spectrometer

Atomic layer deposition (ALD) is currently a widespread method to grow conformal thin films with a sub-nm thickness control. By using ALD for nanolaminate oxides, it is possible to fine tune the electrical, optical and mechanical properties of thin films. In this study the elemental depth profiles and surface roughnesses were determined for Al₂O₃ + TiO₂ nanolaminates with nominal single-layer thicknesses of 1, 2, 5, 10 and 20 nm and total thickness between 40 nm and 60 nm. The depth profiles were measured by means of a time-of-flight elastic recoil detection analysis (ToF-ERDA) spectrometer recently installed at the University of Jyväskylä. In TOF-E measurements ⁶³Cu, ³⁵Cl, ¹²C and ⁴He ions with energies ranging from 0.5 to 10 MeV, were used and depth profiles of the whole nanolaminate film could be analyzed down to 5 nm individual layer thickness.     

The thermoluminescent properties of lithium triborate (LiB3O5) activated by aluminium

In this paper, the thermoluminescence (TL) dosimetric characteristics of Al-doped LiB₃O₅ compounds are presented. The powder samples were prepared by the solid-state reaction method and the formation of the compounds were confirmed by an X-ray diffraction study. The TL studies of undoped and Al-doped LiB₃O₅ samples showed similar glow curve structures. They have three TL glow peaks at about 60, 130 and 200 °C after heating at a constant heating rate of 1 °C/s. Their comparative TL studies indicated that 5 wt% Al-doped LiB₃O₅ compound was approximately 240 times more sensitive than undoped compound. The TL emission spectra of Al-doped LiB₃O₅ showed a maximum band at around 520 nm. The main dosimetric characteristics, which are namely the TL dose response, TL sensitivity, fading, minimum detectable dose, reproducibility, precision of dose measurement and annealing procedure, indicated that Al-doped LiB₃O₅ sample, can be used in dosimetric applications. The trap parameters namely order of kinetics (b), activation energy (E) and frequency factor (s) associated with the glow peaks in beta irradiated undoped and Al-doped LiB₃O₅ samples were obtained by glow curve deconvolution (GCD) program.     

Temperature effect study of silicon-on-insulator structures prepared by high dose implantation of nitrogen

The temperature effect on the microstructure of the N⁺-ion implantation-induced Si₃N₄ buried layer was investigated. The underlying silicon nitride layers were formed in a Si (1 1 1) wafer after implantation of 50 keV nitrogen ions (fluence: 1 × 10¹⁷, 2 × 10¹⁷ and 5 × 10¹⁷ ions/cm²). It was observed that a continuous amorphous layer of about 200 nm thickness was formed in all implanted samples due to the irradiation damage. After 30 min annealing at 900 °C, poly-crystalline Si₃N₄ products were found by TEM examination in the specimen implanted with 5 × 10¹⁷ ions/cm² dose. In the case of annealing at 1200 °C a continuous single-crystalline α-Si₃N₄ buried layer was formed indicating that the amorphous layer in the implanted samples could be transformed into three successive layers, which are amorphous SiO₂, single-crystal α-Si₃N₄ and retained defects from surface to inner substrate, respectively.     

N-TiO2 nanoparticles embedded in silica prepared by Ti ion implantation and annealing in nitrogen

Room-temperature Ti ion implantation and subsequent thermal annealing in N₂ ambience have been used to fabricate the anatase and rutile structured N-doped TiO₂ particles embedded in the surface region of fused silica. The Stopping and Range of Ions in Matter (SRIM) code simulation indicates a Gaussian distribution of implanted Ti, peaked at ∼75 nm with a full width at half maximum of ∼80 nm. However, the transmission electron microscopy image shows a much shallower distribution to depth of ∼70 nm. Significant sputtering loss of silica substrates has occurred during implantation. Nanoparticles with size of 10-20 nm in diameter have formed after implantation. X-ray photoelectron spectroscopy indicates the coexistence of TiO₂ and metallic Ti in the as-implanted samples. Metallic Ti is oxidized to anatase TiO₂ after annealing at 600 °C, while rutile TiO₂ forms by phase transformation after annealing at 900 °C. At the same time, N-Ti-O, Ti-O-N and/or Ti-N-O linkages have formed in the lattice of TiO₂. A red shift of 0.34 eV in the absorption edge is obtained for N-doped anatase TiO₂ after annealing at 600 °C for 6 h. The absorbance increases in the ultraviolet and visible waveband.     

A track structure model of optically stimulated luminescence from Al2O3:C irradiated with 10-60 MeV protons

We investigated the optically stimulated luminescence (OSL) signal from Al₂O₃:C irradiated with 10-60 MeV protons to estimate the potential use of this material as a proton dosimeter. After irradiation, OSL decay curves were read out and we used both the initial part and the total area of these curves as response signal. A precondition for optimal proton dosimetry is an LET-independent response and the experimental data showed such an independence at 0.3 Gy for the initial OSL signal.To understand the experimental results, we applied target and track structure theory. Here, the OSL signal is considered to be a result of target activation and the OSL proton signal is calculated from the OSL gamma signal and a radial dose distribution around the proton track. Although several simplifications were made to ease calculations, the classic track structure theory can qualitatively account for all the main features of the experimental data. We estimate a target radius to be between 30 and 150 nm and associate this radius with a charge migration distance in the crystal.The model calculations suggest that the dose and LET-dependency of the OSL signal is a result of an unique mixture of one- and two-hit targets. This implies that the initial OSL signal from Al₂O₃:C in general is not LET-independent at 0.3 Gy or lower doses. However, a mixture of the initial and total OSL signal could provide an LET-independent response in a given LET and dose interval.     

Effects of Mg-ion implantation in α-Al2O3 and α-Al2O3:Mg crystals: Electrical conductivity and electronic structure changes

Undoped and Mg-doped α-Al₂O₃ single crystals were implanted with Mg ions, with an energy of 90 keV and a fluence of 10¹⁷ ions/cm². DC electrical measurements using the four-point probe method, between 295 and 428 K, were used to characterize the electrical conductivity of the implanted area. Measurements in this temperature range indicate that the electrical conductivity after implantation is thermally activated with an activation energy of about 0.03 eV both in undoped and in reduced Mg-doped α-Al₂O₃ crystals, whereas the activation energy in oxidized Mg-doped α-Al₂O₃ crystals remains close to that before implantation. The I-V characteristics of the latter samples reveal a blocking behavior of the electrical contacts on the implanted area in contrast to the ohmic contacts observed in α-Al₂O₃ single crystals with the c-axis perpendicular to the broad face, where the Mg ions were implanted. We conclude that the enhancement in conductivity observed in the implanted regions is related to the intrinsic defects created by the implantation, rather than to the implanted Mg ions. The relationship between the oxygen vacancy concentrations at different stages of etching and the changes in the electronic structure, the chemical bonding, and the Al³⁺(2p)/O²⁻(1s) and Mg²⁺(1s)/O²⁻(1s) relative intensities was studied by X-ray Photoemission Spectroscopy.     

Development and characterisation of a new ODS ferritic steel for fusion reactor application

This paper describes the microstructure, tensile properties and Charpy impact resistance of a reduced activation oxide dispersion strengthened ferritic steel Fe-14Cr-2W-0.3Ti-0.3Y₂O₃ produced by mechanical alloying of a pre-alloyed, gas atomised steel powder with Y₂O₃ particles, compaction by hot extrusion at 1100 °C, hot rolling at 700 °C and heat treatment at 1050 °C for 1 h. At room temperature the material exhibits a high ultimate tensile strength of about 1420 MPa and high yield strength of about 1340 MPa in the transverse direction. In the longitudinal direction the values are about 10% lower, due to the anisotropy of the microstructure (elongated grains in the rolling direction). At 750 °C the material still exhibits relatively high yield strengths of about 325 MPa and 305 MPa in the longitudinal and transverse directions, respectively. The material exhibits reasonable uniform and total elongation values over the temperature range 23-750 °C, in both transverse and longitudinal directions. The material exhibits weak Charpy impact properties in the transverse direction. Charpy impact properties are slightly better in the longitudinal direction, with upper shelf energy of about 4.2 J and a ductile-to-brittle transition temperature of about 8.8 °C.     

Corrosion behavior of Al-surface-treated steels in liquid Pb-Bi in a pot

Corrosion tests were performed in oxygen-saturated liquid Pb-Bi at 450 °C and 550 °C in a pot for 3000 h for Al-surface-treated steels containing various levels of Cr contents. The Al surface treatments were achieved using a gas diffusion method and a melt dipping method. Al₂O₃, FeAl₂ and AlCr₂ produced by the gas diffusion method exhibited corrosion resistance to liquid Pb-Bi, while the surface layer produced by the melt dipping method suffered a severe corrosion attack. Fe₄Al₁₃ and Fe₂Al₅ produced by the melt dipping method disappeared during the corrosion test at 550 °C and only FeAl remained.     

Preparation and characterization of lithium-titanate pebbles by solid-state reaction extrusion and spherodization techniques for fusion reactor

For the development of TBM for fusion reactors, lithium containing ceramics as against the metal are preferred as tritium breeding material. Lithium titanate (Li₂TiO₃) is one such chosen ceramic tritium breeder. Li₂TiO₃ pebbles are conventionally prepared by sol-gel process and wet process. Solid state reaction of lithium carbonate with titanium dioxide is preferred route for the bulk production of Li₂TiO_3. Thermo-gravimetric and differential thermal analysis (TG-DTA) techniques have been used in the present study to understand the solid state reaction of intimate mixture of lithium carbonate and titanium dioxide. It was found out that single phase lithium titanate (Li₂TiO₃) is produced at 750 °C and the reaction is completed in 6 h. Fine powders of lithium titanate obtained after milling and classification were mixed with aqueous solution of PVA to prepare green pebbles of desired size and shape. The pebbles were subsequently sintered at 900 °C and the effect of sintering time on the properties of sintered pebbles was studied. The reaction mechanisms and the product qualities obtained by the solid state reaction, extrusion and spherodization techniques are discussed in this paper.     

Ion beam induced modifications in electron beam evaporated aluminum oxide thin films

Al₂O₃ thin films find wide applications in optoelectronics, sensors, tribology etc. In the present work, Al₂O₃ films prepared by electron beam evaporation technique are irradiated with 100 MeV swift Si⁷⁺ ions for the fluence in the range 1 × 10¹² to 1 × 10¹³ ions cm⁻² and the structural properties are studied by glancing angle X-ray diffraction. It shows a single diffraction peak at 38.2° which indicates the γ-phase of Al₂O₃. Further, it is observed that as the fluence increases up to 1 × 10¹³ ions cm⁻² the diffraction peak intensity decreases indicating amorphization. Surface morphology studies by atomic force microscopy show mean surface roughness of 34.73 nm and it decreases with increase in ion fluence. A strong photoluminescence (PL) emission with peak at 442 nm along with shoulder at 420 nm is observed when the samples are excited with 326 nm light. The PL emission is found to increase with increase in ion fluence and the results are discussed in detail.     

Ion guiding through capillaries in uncoated Al2O3 membranes

We made an experimental study on ion guiding through capillaries in uncoated Al₂O₃ membranes using a variety of ions such as O¹⁺, O³⁺, and O⁶⁺. The incident energy was varied within the range of 30-150 keV. The results were compared with others using coated PET and Al₂O₃ capillary membranes as well as with the so-called scaling law discovered by Stolterfoht and his co-workers. Good agreement of our results with the scaling law was found. However, our membranes showed extraordinarily strong guiding ability. The reason lies in that our membranes were uncoated. A slower charge drift speed along the insulating capillary wall and a much larger equilibrium charge Q_∞ seems to exist in our experiment.     

Vacuum plasma etching of 1 wt% La2O3 dispersed tungsten

Vacuum plasma etching of 1 wt% La₂O₃ doped tungsten alloy surfaces were carried out to refine the surface morphology for enhancing its bonding characteristics with copper for fusion reactor components. Three different gas compositions containing argon with zero, 14.3 and 25 vol% hydrogen were used to carry out the plasma etching from 30 to 120 s on the given samples. Mitutoyo surface roughness (R_a) measurement, FORM TALYSURF and scanning electron microscopy (SEM) were employed to measure the changes in the surface roughness. Plasma etching with 14.3 vol% hydrogen mixture was found to be the best in micro-roughening the alloy surface. The maximum increase of 44% in R_a value was obtained with this gas mixture, when etched for 90 s.     

Thermal–hydraulics features of the use of LEU U3Si2 fuel in low-power reactors

Calculations for the use of the U₃Si₂ LEU fuel in low-power research reactors were made. The design basis accident was simulated using the feedback coefficients calculated by the BMAC system. Usability of this fuel in low-power research reactors was demonstrated for both normal daily and accidental operation conditions even if the power of the reactor touches 142 kW during the design basis accident simulation. Both HEU and LEU fuels behave similarly in the normal operation, the temperature of the cladding reaching about 60 °C while higher temperature are obtained for the accidental conditions in the case of the LEU fuel (about 113.7 °C against 98.6 °C for the fuel center temperatures).     

Recovery of neutron-irradiation-induced defects of Al2O3, Y2O3, and yttrium-aluminum garnet

SiC fiber-reinforced SiC matrix composites (SiC_f/SiC) are considered as one of the candidates for blanket materials in future fusion reactors and as an advanced fuel cladding material for next-generation fission reactors. Generally, the densification of SiC needs sintering additives and oxides such as Al₂O₃, Y₂O₃, and yttrium-aluminum garnet (YAG, Y₃Al₅O₁₂), which are frequently added to SiC. However, the effects of neutron irradiation on sintering additives are still unclear. In this study, we performed the neutron irradiation of Al₂O₃, Y₂O₃, and YAG at fluences up to 2.0–2.5 × 10²⁴ n/m² (E > 0.1 MeV) at 60–90 °C. The isochronal recovery of the macroscopic volume of Al₂O₃ against annealing temperature showed smooth and continuous shrinkage at a temperature of up to 1200 °C, and the volume slightly increased above that temperature. In contrast, the volume of Y₂O₃ showed quick shrinkage at the low temperature range, and slower and smooth recovery was observed up to ～1100 °C. In the case of YAG, the recovery of volume occurred in a step-wise manner at 600–750 °C, and continuous shrinkage occurred at temperatures lower and higher than that temperature range. The activation energies for the macroscopic volume recoveries of three oxides were obtained from the Arrhenius plots of the rate coefficients. Two-stage recovery was observed for Al₂O₃, whereas more complicated recovery processes were suggested for Y₂O₃ and YAG.