The effect of pre-irradiation annealing on the thermoluminescence of LiF:Mg,Cu, P phosphor grown by EFG technique

LiF crystal doped with magnesium (Mg), copper (Cu) and phosphorous (P) was grown in the form of multicrystalline sheet using Edge-defined film-fed growth (EFG) technique for dosimetry application. These crystals were grown in argon gas atmosphere using graphite crucible and stainless steel die. Dosimetry peak was observed at 210 °C for as-grown crystal. As reported earlier LiF:Mg, Cu, P is a highly sensitive material but losses its sensitivity if annealed at temperature above 240 °C. In this paper, the effect of annealing temperature on thermoluminescence glow-curve structure, maximum peak temperature, peak height and integrated area of the glow peak of EFG grown samples was investigated in detail. Annealing temperature range from 220 °C to 500 °C was considered for the study. Experimental results of the obtained glow curve show that with increase in annealing temperature, glow peak shift towards higher temperature region with substantial increase in TL intensity. Annealing at 500 °C for 10 min gave maximum TL intensity with main dosimetry peak positioned at 233 °C. Change in the defect structure with different pre-annealing temperature was analysed using trapping parameters.     

Newly developed highly sensitive LiF:Mg,Cu,Si TL discs with good stability to heat treatment

The preparation method and some dosimetric properties of the new LiF:Mg,Cu,Si discs are presented. The effect of heat treatments on LiF:Mg,Cu,Si was investigated. The shape of the glow curve for LiF:Mg,Cu,Si is similar to that for standard LiF:Mg,Cu,P (GR-200A), and shows minimal differences when annealed in the range from 260 °C to 290 °C for 10 min. The TL sensitivity for LiF:Mg,Cu,Si is much lower than that for GR-200A, but is 35 times larger than that for TLD-100 and is slightly higher than that for HMCP. The height of the high-temperature peaks for LiF:Mg,Cu,Si is not only lower than that for GR-200A, but also lower than that for HMCP. The glow curve shape of LiF:Mg,Cu,Si annealed at 260 °C for different times shows minimal differences and TL response remains stable. These results indicate that the new LiF:Mg,Cu,Si disc has a good stability to thermal treatments and a lower residual TL signal.     

The reusability characteristics of LiF:Mg,Cu,P with a maximum intensity at 280 °C in an environment with elevated temperature

Efforts are aimed at finding a method that could serve TL dosimetric measurements in the range of low-dose but carried out in an environment with elevated temperature. The temperature at the position of the maximum intensity of LiF:Mg,Cu,P was about 280 °C when annealed at 460 °C. LiF:Mg,Cu,P with a maximum intensity at 280 °C should present good thermal stability. The TL intensity of LiF:Mg,Cu,P with a maximum intensity at 280 °C was about 54% of the standard LiF:Mg,Cu,P, it should have a minimum measurable dose in the range of micro-Gy. LiF:Mg,Cu,P with a maximum intensity at 280 °C could be re-used by the 660 °C/30 min annealing, followed by 270 °C/20 min, 240 °C/10 min and 460 °C/30 min. It's possible for LiF:Mg,Cu,P to be extended application for low dose test in an environment with elevated temperature.     

Investigations of thermoluminescence properties of multicrystalline LiF: Mg,Cu, Si phosphor prepared by edge defined film fed growth technique

Thermoluminescence (TL) properties of LiF: Mg, Cu, Si phosphor prepared in multicrystalline form using edge defined film fed growth (EFG) technique has been investigated. The effect of preparation route on TL properties and thermal stability has been studied. To improve the TL dosimetry properties, phosphor is subjected to different annealing temperatures ranging from 250 °C to 450 °C. The shape of the glow curve structure and peak temperature remains similar at different annealing temperatures, however peak intensities vary. The consistency in the glow curve structure with annealing temperature elucidate that TL trapping states are stable in nature. Thermal annealing at 300 °C for 10 min gives maximum TL intensity with main dosimetry peak at 209 °C. The TL intensity of the main dosimetry peak is increased by a factor of five as compared to as-grown crystal. The thermal stability of LiF: Mg, Cu, Si is found to be better than LiF: Mg, Cu, P. Trapping parameters are calculated to have an insight study of defect states. A simple glow curve structure, tissue equivalency, thermal stability, low residual signal, linear response and reusability makes LiF: Mg, Cu, Si a suitable phosphor for radiation therapy, radio diagnostics and personnel dosimetry applications.     

Optimization of preparation procedure of LiF:Mg,Cu,Si TLD for improving the reusability

Several thermal treatments in the temperature range from 270 °C to 320 °C (each of 10 min) were tested as a final preparation procedure of LiF:Mg,Cu,Si to improve the protocol of TL readout with less residual signal for the LiF:Mg,Cu,Si TLD. This high sensitivity LiF:Mg,Cu,Si TLD exhibited thermal stability much better than that of the well known LiF:Mg,Cu,P. For LiF:Mg,Cu,Si, a readout temperature up to 300 °C did not affect the TL sensitivity and glow curve structure for 12 cycles of exposure and readout following an initial thermal treatment at 295 °C for 10 min. The residual TL signal also remained negligible.     

The dependence of thermoluminescence of LiF:Mg,Cu,Si on sintering temperatures and dopants concentrations

The dependence of thermoluminescence (TL) of LiF:Mg,Cu,Si on sintering temperatures and dopants concentrations were investigated. The dependency of the TL in LiF:Mg,Cu,Si on sintering temperature exhibits a very sharp maximum at 830 °C. LiF:Mg,Cu,Si is much too sensitive than LiF:Mg,Cu,P to sintering temperature. The glow curve and the TL sensitivity depend on the concentration of Mg, Cu and Si, showing a distinct maximum for certain concentrations of these impurities. Mg seems to be the most essential dopant, as very small changes of the Mg content strongly influence both the glow curve and the TL sensitivity. Si is the main activator responsible for TL emission. The stability to heat treatments in LiF:Mg,Cu,Si was influenced greatly by Mg concentrations. The thermal instability in LiF:Mg,Cu,Si is caused not by Cu and Si but Mg ion state change. It was found that the optimum concentrations are Mg:0.6 mol%, Cu:0.03 mol% and Si:0.9 mol% for this material, which showed the best stability to heat treatment.     

Influence of sintering temperatures on LiF:Mg,Cu,P with various magnesium concentrations

The dependence of LiF:Mg,Cu,P samples with various concentrations of Mg on sintering temperatures was investigated to find a new dosimeter. The influence of high sintering temperatures on LiF:Mg,Cu,P chips depends strongly on Mg concentrations. The height of the main peak versus the sintering temperatures exhibits a maximum, the position of which varies between 690 °C and 750 °C, depending on the Mg concentration in the range studied. The high temperature peaks of LiF:Mg,Cu,P for various Mg concentrations reduce basically when the sintering temperature is increased. LiF:Mg,Cu,P is much less sensitive than LiF:Mg,Cu,Si to sintering temperature. LiF:Mg,Cu,P with 0.6 mol% of Mg can be re-used at annealing temperature of 260 °C, regardless of the sintering temperature. It was found that the optimum concentration is Mg: 0.6 mol%, the optimum sintering temperature is 750 °C, considering that LiF:Mg,Cu,P with a low residual signal and good sensitivity can be re-used at annealing temperature of 260 °C and produced in a large scale. The new optimum LiF:Mg,Cu,P formation has 52 times higher than that of the TLD-100, and an extremely low residual signal of 0.07% without an initialization readout procedure.     

Long term study of Harshaw TLD LiF – LLD and uncertainty

Long term study of Harshaw TLD LiF has been performed in this work. The study is carried out over a period of 24 months at storage temperatures of 0 °C, 20 °C and 40 °C using more than 3500 dosimeters. The length and variations of this study may be the most comprehensive study published to date. The dosimeters are HarshawTLD LiF based cards and extremity dosimeters, which include LiF:Mg,Ti and LiF:Mg,Cu,P materials in their different isotopes, sizes and forms. There are three parts in this study: material fade in sensitivity and in signal; lower limit of detection (LLD) and uncertainty; and glow curve peaks and sensitivity change over 24 months. Part I was presented at the SSD15 (15th International Conference on Solid State Dosimetry) in Delft. This paper is the continuous work focused on Part II – the lower limit of detection and uncertainty analysis. The detailed results of each case are provided.     

Thermoluminescence,photoluminescence and EPR studies on Mn2+ activated yttrium aluminate (YAlO3) perovskite

Thermoluminescence (TL) measurements were carried out on undoped and Mn²⁺ doped (0.1 mol%) yttrium aluminate (YAlO₃) nanopowders using gamma irradiation in the dose range 1–5 kGy. These phosphors have been prepared at furnace temperatures as low as 400 °C by using the combustion route. Powder X-ray diffraction confirms the orthorhombic phase. SEM micrographs show that the powders are spherical in shape, porous with fused state and the size of the particles appeared to be in the range 50–150 nm. Electron Paramagnetic Resonance (EPR) studies reveal that Mn ions occupy the yttrium site and the valency of manganese remains as Mn²⁺. The photoluminescence spectrum shows a typical orange-to-red emission at 595 nm and suggests that Mn²⁺ ions are in strong crystalline environment. It is observed that TL intensity increases with gamma dose in both undoped and Mn doped samples. Four shouldered TL peaks at 126, 240, 288 and 350 °C along with relatively resolved glow peak at 180 °C were observed in undoped sample. However, the Mn doped samples show a shouldered peak at 115 °C along with two well defined peaks at ～215 and 275 °C. It is observed that TL glow peaks were shifted in Mn doped samples. The kinetic parameters namely activation energy (E), order of kinetics (b), frequency factor (s) of undoped, and Mn doped samples were determined at different gamma doses using the Chens glow peak shape method and the results are discussed in detail.     

The glow curve structure for the LiF:Mg,Cu,Na,Si TL detector with dopants concentrations and sintering temperatures

The glow curve structures for LiF:Mg,Cu,Na,Si TL detectors with various dopant concentrations and sintering temperatures were investigated for the improvement of the glow curve structure and sensitivity of the TL detector. The dopant concentrations were varied over the following ranges: Mg (0–0.25 mol%), Cu (0–0.07 mol%), Na and Si (0–1.5 mol%). With increasing Cu concentration, the intensity of the main peak was intensified and reached a maximum at a concentration of 0.05 mol%. The high-temperature peak was reduced. The dependency of the main peak intensity on the Mg concentration exhibits a sharp maximum at 0.2 mol%. The intensity of the high-temperature peak tends to rise slightly with increasing Mg concentration. It was found that the optimum concentrations of the dopants in the LiF:Mg,Cu,Na,Si TL material are Mg: 0.2 mol%, Cu: 0.05 mol%, Na and Si: 0.9 mol%. The dependency of the main peak intensity on sintering temperature exhibits a very sharp maximum at 830°C. The high-temperature peak was rapidly reduced after 825°C.     

Effect of pre-annealing on NO32- centers in synthetic hydroxyapatite

Effect of pre-annealing of synthetic hydroxyapatite (HAP) on properties of γ- and UV- induced NO₃^2- centers was studied by electron paramagnetic resonance (EPR). Nitrate-containing hydroxyapatite powders ((N)HAP)) and the powders with an admixture of carbonate and nitrate ions ((C,N)HAP) were annealed in the temperature range T_ann = 20 °C ? 600 °C before irradiation. It was found that pre-annealing of (N)HAP samples changes the parameters of NO₃^2- centers while no changes took place in (C,N)HAP. Moreover, at the pre-annealing temperatures T_ann > 200 °C two new NO₃^2- centers were observed in (N)HAP samples; they are characterized by larger value of A_⊥ (3.67 and 4.41 mT) as compared to the known centers. It was also found that the dependence of NO₃^2- centers amount on T_ann is non-monotonous in both types of samples. Presumably this is caused by the escape of water molecules from HAP during the annealing and essential modification of the defect subsystem of HAP.     

Electric field effect on the luminescence of KI:T1

Thermoluminescence of KI: T1, X- or β-irradiated at T ?77°K shows two main peaks at 105°K and 170°K. They are respectively attributed to the recombination of mobile V_K centres with T1^O centres and to the recombination of thermally released electrons from T1^O centres with T1²⁺ centres. Similar experiments performed under static electric fields (E <40kV cm^-1) show that the intensity of the second glow peak is strongly reduced. The relative intensity variation is anticorrelated with the intensity of glow peaks occurring at T > 230 °K. We suggest that in the temperature range in which T1^O centres are thermally ionised, the effect of the electric field is to favour the retrapping of these electrons on other traps (still unknown). Irradiation doses also play an important role and their effects are studied at T = 77 °K and T = 200 °K.     

Thermoluminescence studies of thermally treated CaB4O7:Dy

Borate based thermoluminescence dosimeters (TLD) show high sensitivity and good TL characteristics. One of the promising material amongst the dosimeters is Dy doped CaB₄O₇. Spectrally resolved thermoluminescence of Dy doped CaB₄O₇ shows three glow peaks at about 50 °C, 240 °C and 380 °C, the intensity of the 240 °C glow peak being the maximum. All TL experiments were conducted on a high sensitivity TL spectrometer at Sussex University with a heating rate of 50 °C min^?1. Two main emissions associated with the Dy dopant are observed at ～480 and 580 nm. The samples were subjected to a series of treatments including excitation by X-rays and UV laser radiation. As part of the present research CaB₄O₇:Dy materials were subjected to two different heat treatments; quenching and slow cooling in order to investigate the changes in TL characteristics.     

Effect of 100 MeV swift Si8+ ions on structural and thermoluminescence properties of Y2O3:Dy3+nanophosphor

Nanoparticles of Y₂O₃:Dy³⁺ were prepared by the solution combustion method. The X-ray diffraction pattern of the 900°C annealed sample shows a cubic structure and the average crystallite size was found to be 31.49?nm. The field emission scanning electron microscopy image of the 900°C annealed sample shows well-separated spherical shape particles and the average particle size is found to be in a range 40?nm. Pellets of Y₂O₃:Dy³⁺ were irradiated with 100?MeV swift Si⁸⁺ ions for the fluence range of 3?×?10^11_3?×?10¹³ ions cm^?2. Pristine Y₂O₃:Dy³⁺ shows seven Raman modes with peaks at 129, 160, 330, 376, 434, 467 and 590?cm^?1. The intensity of these modes decreases with an increase in ion fluence. A well-resolved thermoluminescence glow with peaks at ～414?K (T_m1) and ～614?K (T_m2) were observed in Si⁸⁺ ion-irradiated samples. It is found that glow peak intensity at 414?K increases with an increase in the dopant concentration up to 0.6?mol% and then decreases with an increase in dopant concentration. The high-temperature glow peak (614?K) intensity linearly increases with an increase in ion fluence. The broad TL glow curves were deconvoluted using the glow curve deconvoluted method and kinetic parameters were calculated using the general order kinetic equation.     

Post-irradiation storage and thermal stability of thermoluminescence glow peaks in LiF:Mg,Cu,Si

Newly developed LiF:Mg,Cu,Si was found to exhibit no significant fading on room temperature post-irradiation storage up to several months. In view of the wide variation in the reported data of fading of LiF:Mg,Cu,P exhibiting glow curve structure similar to that of LiF:Mg,Cu,Si, a study of the effect of post-irradiation storage and thermal treatments on the deconvoluted glow peaks of LiF:Mg,Cu,Si was undertaken. The decay of inseparable peak-3 by post-irradiation storage or thermal treatments did not indicate any rearrangement in the trap occupation that would affect the response of the main peak (peak-4). A post-irradiation treatment at 125 °C for 10 min was found to be the optimum to eliminate the lower temperature peaks.     

Sputtered magnesium diboride thin films: Growth conditions and surface morphology

Magnesium diboride (MgB₂) thin films were deposited on C-plane sapphire substrates by sputtering pure B and Mg targets at different substrate temperatures, and were followed by in situ annealing. A systematic study about the effects of the various growth and annealing parameters on the physical properties of MgB₂ thin films showed that the substrate temperature is the most critical factor that determines the superconducting transition temperature (T_c), while annealing plays a minor role. There was no superconducting transition in the thin films grown at room temperature without post-annealing. The highest T_c of the samples grown at room temperature after the optimized annealing was 22 K. As the temperature of the substrate (T_s) increased, T_c rose. However, the maximum T_s was limited due to the low magnesium sticking coefficient and thus the T_c value was limited as well. The highest T_c, 29 K, was obtained for the sample deposited at 180 °C, annealed at 620 °C, and was subsequently annealed a second time at 800 °C. Three-dimensional (3D) AFM images clearly demonstrated that the thin films with no transition, or very low T_c, did not have the well-developed MgB₂ grains while the films with higher T_c displayed the well-developed grains and smooth surface. Although the T_c of sputtered MgB₂ films in the current work is lower than that for the bulk and ex situ annealed thin films, this work presents an important step towards the fabrication of MgB₂ heterostructures using rather simple physical vapor deposition method such as sputtering.     

Thermal annealing of GaSb quantum dots in GaAs formed by droplet epitaxy

We investigate effects of annealing on GaSb quantum dots (QDs) formed by droplet epitaxy. Ga droplets grown on GaAs are exposed to Sb molecular beam and then annealed at T_a=340–450 °C for 1 min to form GaSb QDs. An atomic force microscope study shows that with the increase of T_a, the average diameter of dots increases by about 60%, while their density decreases to about 1/3. The photoluminescence (PL) of GaSb QDs is observed at around 1 eV only for those samples annealed above T_a=380 °C, which indicates that the annealing process plays an important role in forming high quality GaSb QDs.     

Thermoluminescence and optically stimulated luminescence characteristics of Al2O3 doped with Tb

In the present work policrystals of α − Al₂O₃ doped with terbium were synthesized using the solvent evaporation method. The samples were prepared using Al(NO₃)₃·9H₂O and Tb(NO₃)₃·5H₂O reagents, with Tb concentrations between 1 and 5 mol% and thermally treated at high temperature above ∼1400 °C. X-ray diffraction measurements showed the α-phase formation of samples. TL glow curve presented an intense peak at ∼190 °C and two other with low intensity at 290 and 350 °C after gamma irradiation. The best doping concentration which presented high luminescence was the sample doped with 3 mol% of Tb. TL spectra and fluorescence measurements showed similar luminescence spectra with lines attribute to Tb³⁺ ions. A linear behavior to gamma dose between 1 and 20 Gy was observed in TL, using 190 °C peak as well as in OSL signal, this last carried out using 532 nm wavelength stimulation.     

Thermally evaporated CdS/CdTe thin film solar cells: Optimization of CdCl2 evaporation treatment on absorber layer

CdCl₂ treatment is crucial in the fabrication of highly efficient CdS/CdTe thin-film solar cells. This study reports a comprehensive analysis of thermal evaporated CdS/CdTe thin-film solar cells when the CdTe absorber layer is CdCl₂ annealed at temperatures from 340 to 440 °C. Samples were characterized for structural, optical, morphological and electrical properties. The films annealed at 400 °C showed better crystallinity with a cubic zinc blende structure having large grains. Higher refractive index, optical conductivity, and absorption coefficient were recorded for the CdTe films annealed at 400 °C with CdCl₂. Optimum photoactive properties for CdS/CdTe thin-film solar cells were also obtained when samples were annealed at 400 °C for 20 min with CdCl₂, and the best device exhibited V_OC of 668.4 mV, J_SC of 13.6 mA cm⁻², FF of 53.9% and an efficiency of 4.9%.     

A study on thermal degradation of LiF:Mg,Cu,P and LiF:Mg,Cu,Si

We investigated the thermal degradation of LiF:Mg,Cu,P (NTL-250) and LiF:Mg,Cu,Si (MCS) for the development of TL sheet. By thermogravimetry and differential scanning calorimetry (TG-DSC), the exothermic reaction was observed between 320 °C and 400 °C in MCS as well as NTL-250. The heat value of MCS was twice as large as that of NTL-250. This ratio corresponded with that of Mg amount in these TL materials measured by ICP-OES (inductively-coupled plasma optical emission spectrometry). X-ray diffraction (XRD) measurements were also carried out, and the peaks of MgF₂ phase were also observed in degraded MCS sample as well as NTL-250. Moreover, X-ray absorption near-edge structures (XANES) of Cu in these LiF TLDs were measured. The valences of Cu did not change before and after degradation. It indicates that the thermal degradation is caused by not Cu but Mg ion state change. The exothermic reaction is possible caused by the stabilization reactions, and then it was expected to correspond with MgF₂ precipitation. From these results, we concluded that the thermal degradations of these LiF TLDs are caused by the precipitation of MgF₂.