Role of impurities in the thermoluminescence of LiF:Mg,Cu,P

The thermoluminescent properties of lithium fluoride doped with magnesium, copper and phosphorous are reviewed. This material shows specific advantages over LiF (TLD-100) in that is has higher sensitivity, less energy dependence and no supralinear behaviour with dose. However, it suffers from an irreversible loss in sensitivity when heated above 270 degrees C. Possible causes for this loss in sensitivity are discussed and experimental results are shown that indicate potential roles for the Cu, P and O impurities in this process. The present work focuses on the understanding of the impurity contents, inclusions, cluster formation and valence changes in this material by using differential scanning calorimetry (DSC) and glow discharge mass spectroscopy (GDMS). This research concludes that phosphorus inclusions are formed and a valence change of the Cu ions occurs after annealing above 270 degrees C, which degrades the TL sensitivity of LiF:Mg,Cu,P phosphors. It is also shown that a high content of oxygen in the material and control of the oxygen content during processing are critical to maintaining the sensitivity of these phosphors.     

Effect of thermal treatment on carbon-doped silicon oxide low dielectric constant materials

Carbon-doped silicon oxide (SiOCH) low dielectric constant (low-k) material is a good candidate for advanced interconnect technology. Good thermal stability of the dielectric is required due to the many thermal processes involved during IC fabrication. The thermal stability of tetramethylcyclotetrasiloxane (TMCTS) based plasma-enhanced chemical vapor deposition (PECVD) carbon doped low-k material with annealing temperature from 400 to 800 degrees C in N2 was studied. The thermal stability temperature of TMCTS based carbon doped low-k material is 600 degrees C. Above 600 degrees C annealing, the thermal energy can break Si-CH3, Si-C, Si-H, and C-H bonds leading to outgasing, which results in film composition change, weight loss, and thickness shrinkage. Film composition changes, especially carbon loss and oxygen incorporation, can degrade its reliability extremely. Carbon is desorbed in the form of CH4, CO, and other hydrocarbon.     

Blue light stimulated luminescence in calcium fluoride, its characteristics and implications in radiation dosimetry

Strong optically stimulated luminescence (OSL), stimulated by blue light, has been observed, for the first time, in natural calcium fluoride (CaF(2)) phosphor, used as thermoluminescence dosemeters. Traps responsible for all three thermoluminescence (TL) peaks appearing upto 300 degrees C, i.e. 126, 196 and 264 degrees C, were observed to contribute to the blue light stimulated luminescence (BLSL) in CaF(2). When the areas under the respective curves (BLSL and TL) were measured, the BLSL measured at room temperature was found to be approximately 1.8 times the TL output of the dosimetry peak that appeared at approximately 264 degrees C. However, when measured after thermally annealing the first two TL peaks, the BLSL signal was found to be 0.26 times the TL output of the dosimetry peak at 264 degrees C. This paper describes the characteristics of the BLSL signal using linearly modulated OSL after subjecting the phosphor to different annealing treatments. Feasibility studies to assess the usefulness of BLSL in CaF(2) for environmental radiation monitoring are also discussed.     

Thermoluminescence properties of LiMgF3 doped with Ce,Er and Dy

The main dosimetric properties are reported of a new perovskite, LiMgF3, doped with Ce, Er and Dy impurities. An annealing temperature of 400 degrees C for one hour is necessary to erase any previous signal and to stabilise its sensitivity. A readout up to 450 degrees C gives the same result. The glow curve structure consists of two intense and isolated glow peaks at 170 degrees C and 315 degrees C. The sensitivity of both glow peaks to beta irradiation increases as the dopant concentration increases. The sensitivity is higher than that of LiF:Mg,Ti using the glow peaks 4+5 integral. Other properties like TL dose response, fading, sensitivity versus successive readout and ammealing cycles, sensitivity versus the heating rate, sensitivity to light and trapping parameter evaluation were also carried out.     

Application of TL dosemeters for dose distribution measurements at high temperatures in nuclear reactors

Al2O3:Mg,Y ceramic thermoluminescence dosemeters were developed at the Institute of Isotopes for high dose applications at room temperatures. The glow curve of Al2O3:Mg,Y exhibits two peaks--one at 250 degrees C (I) and another peak at approximately 400 degrees C (II). In order to extend the application of these dosemeters to high temperatures, the effect of irradiation temperature was investigated using temperature controlled heating system during high dose irradiation at various temperatures (20-100 degrees C). The new calibration and measuring method has been successfully applied for dose mapping within the hermetic zone of the Paks Nuclear Power Plant even at high temperature parts of blocks.     

Material and sensing properties of Pd-deposited WO3 thin films

The physicochemical and electrical properties of Pd-deposited WO3 thin films were investigated as a function of Pd thickness, annealing temperature, and operating temperature for application as a hydrogen gas sensor. WO3 thin films were deposited on an insulating material using a thermal evaporator. X-ray diffractometry (XRD), field emission scanning electron microscopy (FE-SEM), atomic force microscopy (AFM), and X-ray photoelectron spectroscopy (XPS) were used to evaluate the crystal structure, microstructure, surface roughness, and chemical property of the films, respectively. The deposited films grew into polycrystalline WO3 with a rhombohedral structure after annealing at 500 degrees C. Adding Pd had no effect on the crystallinity, but suppressed the growth of WO3 grains. The Pd was scattered as isolated small spherical particles of PdO2 on the WO3 thin film after annealing at 500 degrees C, while it agglomerated as irregular large particles or diffused into the WO3 after annealing at 600 degrees C. PdO2 reduction under H2 and reoxidation under air were dependent on both the Pd deposition thickness and annealing conditions. The WO3 thin film with a 2-nm-thick Pd deposit showed a good response and recovery to H2 gas at a 250 degrees C operating temperature.     

Preparation,dosimetric characterisation and investigation of related TSL defect centres in Li3Po4:Mg,Cu phosphor

L3PO4:Mg,Cu, a low effective atomic number and high sensitivity TSL phosphor, has been prepared. Its TSL glow curve shows a major peak around 360 degrees C with minor peaks around 110 degrees C and 230 degrees C. The optimum concentrations of the dopants are found to be 200 ppm each. Its gamma sensitivity is 1.2 times as compared to CaSO4:Dy (0.1 mol%). The optimum preirradiation annealing treatment is found to be 650 degrees C, 15 min. Its PL emission shows a band at 370 nm with excitation band at 250 nm. Dose to TSL response shows that its response is linear up to the gamma dose of 100 Gy for irradiations carried out at RT. An irradiated sample shows a distinct new ESR signal, which is tentatively assigned to an electron/hole localised on one of the oxygen(s) of the phosphate group. Step annealing experiments show decay of the defect centre around 340 degrees C. This correlates well with the TSL peak around 360 degrees C.     

Thin transparent W-doped indium-zinc oxide (WIZO) layer on glass

Annealing effect on structural and electrical properties of W-doped IZO (WIZO) films for thin film transistors (TFT) was studied under different process conditions. Thin WIZO films were deposited on glass substrates by RF magnetron co-sputtering technique using indium zinc oxide (10 wt.% ZnO-doped In2O3) and WO3 targets in room temperature. The post annealing temperature was executed from 200 degrees C to 500 degrees C under various O2/Ar ratios. We could not find any big difference from the surface observation of as grown films while it was found that the carrier density and sheet resistance of WIZO films were controlled by O2/Ar ratio and post annealing temperature. Furthermore, the crystallinity of WIZO film was changed as annealing temperature increased, resulting in amorphous structure at the annealing temperature of 200 degrees C, while clear In2O3 peak was observed for the annealed over 300 degrees C. The transmittance of as-grown films over 89% in visible range was obtained. As an active channel layer for TFT, it was found that the variation of resistivity, carrier density and mobility concentration of WIZO film decreased by annealing process.     

The application of computerised analysis of glow curves to personal dosimetry in LiF:Mg,Cu,P

In personnel monitoring services, it is important to omit the high-temperature annealing process so that large numbers of TL detectors can be produced economically. There are two efficient ways of reducing the residual signal of LiF:Mg,Cu,P. One is by increasing the maximum readout temperature and the other is by improving the preparation procedure (increasing the Cu concentration and the sintering temperature) but both reduce the TL sensitivity. In personal dosimetry the real dosimetric signals are separated from the residual signals by computerised analysis of glow curves. The adverse influence of the high residual signals of LiF:Mg.Cu.P TL material has been effectively eliminated and the sensitivity remains stable. A good dosimetric result using only reader measurement without pre-irradiation oven annealing is attained in a dose range of 50-80,000 microGy.     

Investigation of thermal annealing of optical properties and residual stress of ion-beam-assisted TiO2 thin films with different substrate temperatures

Titanium oxide films were prepared by ion-beam-assisted deposition on glass substrates at various substrate temperatures. The effect of the temperature of thermal annealing from 100 degrees C to 300 degrees C on the optical properties and residual stress was investigated. The influence on the stoichiometry and residual stress of titanium oxides deposited at different substrate temperature was discussed. The residual-stress was minimum and the extinction coefficient was maximum at an annealing temperature of 200 degrees C with a substrate temperature of 150 degrees C. However, when the substrate temperature was increased to 200 degrees C and 250 degrees C, the residual stress was minimum and the extinction coefficient was maximum at an annealing temperature of 250 degrees C. The spectra of x-ray photoelectron spectroscopy reveal that the films lost oxygen and slowly generated lower suboxides at the annealing temperature at which the residual stress was minimum and the extinction coefficient was maximum. As the annealing temperature increased above the temperature at minimum stress, the lower suboxides began to capture oxygen and form stable oxides. TiO2 films deposited at substrate temperatures of 200 degrees C and 250 degrees C were more stable than films deposited at 150 degrees C.     

Development of LiF:Mg,Cu,Si TL material (new KLT-300) with a low-residual signal and high-thermal stability

LiF-based thermoluminescence (TL) materials have been widely used for radiation dosimetry due to their attractive features. LiF:Mg,Cu,P is one of the most sensitive tissue-equivalent TL materials, approximately 40 times more sensitive than LiF:Mg,Ti (TLD-100), but it has two main drawbacks: a thermal loss of the TL sensitivity when annealed at temperatures >240 degrees C, and a relatively high-residual signal. Recently, LiF:Mg,Cu,Na,Si TL material was developed to overcome these drawbacks at the Korea Atomic Energy Research Institute, but it provided only marginal improvements in reducing the residual signal. The newly developed LiF:Mg,Cu,Si TL material has a significantly lower residual signal and a better stability to thermal treatments. In this article, the preparation method and some dosimetric properties (sensitivity and residual signal) of the new LiF:Mg,Cu,Si TL material are presented. At the end of the preparation procedures, a dual-step annealing method is introduced and this has proved as a very efficient method to reduce the high-temperature peak and is the cause of residual signal. Therefore, the high-temperature peak in the glow curve was significantly reduced. The sensitivity is approximately 20 times higher than that of TLD-100 and the residual signal was estimated to be approximately 0.04%.     

Influence of readout parameters on TL response,re-usability and residual signal in LiF:Mg,Cu,P

It has recently been recommended that heating rates do not exceed 10 K.s(-1) and that the maximum temperature of readout should not exceed 265 degrees C for LiF:Mg,Cu,P. In some cases, a decrease of sensitivity in this material in the first of several re-use cycles had been reported. Influence of heating rates up to 30 K.s(-1), duration time up to 40s and maximum readout temperatures up to 270 degrees C on TL response, re-usability and residual signal was investigated. It was found that the maximum readout temperatures above 240 degrees C may lead to the thermoluminscent response decrease in the first several re-use cycles. The readout parameters can be optimised to minimise the residual signal (less than 0.4%) and to retain a constant sensitivity at the same time at high heating rates up to 30 K.s(-1) in a short time (less than 1 min per TL chip) without the necessity of heating above 240 degrees C. A concept of 'efficient residual signal' was put forward to quantify more accurately the real residual signal which affects the precision of the next measurement.     

The influence of post-exposure heating on the stability of MCP-N (LiF:Mg,Cu,P) TL detectors

Post-exposure annealing of highly sensitive LiF:Mg,Cu,P (MCP-N) detectors, at 100 degrees C over 10 or 20 min prior to readout, is usually recommended for routine dosimetry. The purpose of this anneal is to eliminate low-temperature peaks, especially peak 3, which fades at room temperature in about 3 months. However, as this annealing procedure does not entirely eliminate peak 3, 10% of its thermoluminescent (TL) signal still being readable, a fading correction must be applied. The aim of this work was to optimise the conditions of post-exposure treatment, i.e. its temperature and duration, in order to facilitate the use of MCP-N detectors in routine dosimetry. MCP-N detectors were annealed in standard conditions, i.e. at 240 degrees C over 10 min and exposed to a dose of 5 mGy (137Cs). For post-exposure annealing, six different temperatures between 100 degrees C and 150 degrees C and two time periods (10 and 20 min) were tested. TL glow curves were deconvoluted with the GCA code. A post-exposure anneal at 120 degrees C over 10 min was found to be optimal. Heating at this temperature eliminates 100% of the TL signal of peak 3, while maintaining the area and maximum intensity of the main peak 4 unchanged. In this case, no fading correction needs to be applied. Annealing at higher temperatures, up to 150 degrees C, results in a loss of peak 4 signal, and is therefore not recommended.     

Effect of thermal annealing on the optical properties and residual stress of TiO2 films produced by ion-assisted deposition

The effects of thermal annealing of titanium oxide films deposited by ion-beam assistance at annealing temperatures from 100 degrees C to 300 degrees C on the residual stress and optical properties of the films was investigated. The refractive indices and extinction coefficients increased gradually as the temperature was increased from 100 degrees C to 200 degrees C and then declined gradually as the temperature was increased further from 200 degrees C to 300 degrees C. The film lost oxygen and slowly generated lower suboxides as the annealing temperature was reduced below 200 degrees C, as determined by x-ray photoelectron spectroscopy (XPS). As the annealing temperature increased above 200 degrees C, the lower suboxides began to capture oxygen and form stable oxides. XPS measurements were made to verify both the binding energy associated with the Ti 2p line and the variation of the O 1s line. A Twyman-Green interferometer was employed for phase-shift interferometry to study the residual stress. The residual stress declined as the temperature was reduced from 100 degrees C to 200 degrees C because the lower suboxides reduced the stress in the film. Above 200 degrees C, the film began to capture oxygen, so the residual stress rose. At 300 degrees C, the film was no longer amorphous as the anatase was observed by x-ray diffraction.     

Thermoluminescence response of K2YF5:Tb3+ crystals to photon radiation fields

This investigation has been performed to test the feasibility of using K2YF5:Tb3+ crystals as thermoluminescence dosemeters (TLD). K2YF5 single crystals doped with 0.2, 10.0 and 50.0 at.% of trivalent optically active Tb3+ ions as well as K2TbF5 and undoped K2YF5 crystals have been synthesized under hydrothermal conditions. Polished crystal platelets with thickness of about 1 mm have been irradiated with X and gamma rays in order to study thermoluminescent (TL) sensitivity as well as dose and energy response in terms of the Tb3+ concentration in K2YF5. Within this concentration series, K2YF5 crystals doped with 10.0 at.% Tb3+ have been found to have maximum TL response due to a broad asymmetric TL glow peak at 269 degrees C with good linearity of dose response and reproducibility of dose measurements. After deconvolution, the main dosimetric peak has been revealed to be composed of two individual peaks, both with linear TL response behaviour, centered at 210 and 269 degrees C. As it has been proved, the linear TL signal coefficient for K2Y0.9Tb0.1F5 is almost 10 times greater than that for commercial TLD-100 (LiF:Mg,Ti), irradiated with a 137Cs gamma radiation source at the same conditions. The reported results indicate that K2YF5 crystals doped with Tb3+ have potential as promising materials for radiation dosemeters.     

Characteristics and performance of the Sunna high dose dosemeter using green photoluminescence and UV absorption readout methods

Growth in the use of ionising radiation for medical sterilisation and the potential for wide-scale international food irradiation have created the need for robust, mass-producible, inexpensive, and highly accurate radiation dosemeters. The Sunna dosemeter, lithium fluoride injection-moulded in a polyethylene matrix, can be read out using either green photoluminescence or ultraviolet (UV) absorption. The Sunna dosemeter can be mass-produced inexpensively with high precision. Both the photoluminescent and the UV absorption reader are simple and inexpensive. Both methods of analysis display negligible humidity effects, minimal dose rate dependence, acceptable post-irradiation effects, and permit measurements with a precision of nearly 1% 1sigma. The UV method shows negligible irradiation temperature effects from -30 degrees C to +60 degrees C. The photoluminescence method shows negligible irradiation temperature effects above room temperature for sterilisation dose levels and above. The dosimetry characteristics of these two readout methods are presented along with performance data in commercial sterilisation facilities.     

Temperature and pressure-mediated structural transition of ZnS nanoparticles

We demonstrate that the structural transition of ZnS nanoparticles from sphalerite to wurtzite is influenced by high pressures and temperatures. Under the pressure of 1 GPa, the structural transition of ZnS nanoparticles commences at 250 degrees C, much lower than that 400-500 degrees C for ZnS nanoparticles under normal pressures. With the increase of the annealing temperature, the transition is enhanced then inhibited with a maximum transition fraction of 14% at 300 degrees C and disappears at 500 degrees C. At the annealing temperature of 300 degrees C, the structural transition of ZnS nanoparticles keeps almost invariable with the increase of the pressure from 0.6 GPa to 1 GPa. The mechanism for the phenomenon is discussed.     

Effects of temperature on columnar microstructure and recrystallization of TiO2 film produced by ion-assisted deposition

Titanium oxide thin films were deposited by electron-beam evaporation with ion-beam-assisted deposition. The effect of the substrate temperature and annealing temperature on the columnar microstructure and recrystallization of titanium oxide was studied. The values of the refractive index varied from 2.26 to 2.4, indicating that the different substrate temperatures affected the film density. X-ray diffraction revealed that all films were amorphous as deposited. At annealing temperatures from 100 degrees C to 300 degrees C, only the anatase phase was formed. As the substrate temperature increased from 150 degrees C to 200 degrees C to 250 degrees C, the recrystallization temperature fell from 300 degrees C through 250 degrees C to 200 degrees C. Changing the substrate temperature resulted in the formation of various types of columnar microstructure, as determined by scanning-electron microscopy. Different columnar structures resulted in different surface morphologies, as measured by atomic-force microscopy.     

Synthesis,characterization and gas sensing performance of SnO<Subscript>2</Subscript> thin films prepared by spray pyrolysis

In this work, SnO₂ thin films were deposited onto alumina substrates at 350°C by spray pyrolysis technique. The films were studied after annealing in air at temperatures 550°C, 750°C and 950°C for 30 min. The films were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and optical absorption spectroscopy technique. The grain size was observed to increase with the increase in annealing temperature. Absorbance spectra were taken to examine the optical properties and bandgap energy was observed to decrease with the increase in annealing temperature. These films were tested in various gases at different operating temperatures ranging from 50–450°C. The film showed maximum sensitivity to H ₂S gas. The H₂S sensing properties of the SnO₂ films were investigated with different annealing temperatures and H ₂S gas concentrations. It was found that the annealing temperature significantly affects the sensitivity of the SnO₂ to the H ₂S. The sensitivity was found to be maximum for the film annealed at temperature 950°C at an operating temperature of 100°C. The quick response and fast recovery are the main features of this film. The effect of annealing temperature on the optical, structural, morphological and gas sensing properties of the films were studied and discussed.     

Erbium-doped optical fiber fluorescence temperature sensor with enhanced sensitivity,a high signal-to-noise ratio,and a power ratio in the 520-530- and 550-560-nm bands

We analyze and predict the performance of a fiber-optic temperature sensor from the measured fluorescence spectrum to optimize its design. We apply this analysis to an erbium-doped silica fiber by employing the power-ratio technique. We develop expressions for the signal-to-noise ratio in a band to optimize sensor performance in each spectral channel. We improve the signal-to-noise ratio by a factor of 5 for each channel, compared with earlier results. We evaluate the analytical expression for the sensor sensitivity and predict it to be approximately 0.02 degrees C(-1) for the temperature interval from room temperature to above 200 degrees C, increasing from 0.01 degrees C(-1) at the edges of the interval to 0.03 degrees C(-1) at the center, at 100-130 degrees C. The sensitivity again increases at temperatures higher than 300 degrees C, delineating its useful temperature intervals.