Characteristics of TL and PTTL glow curves of gamma irradiated pure Li2B4O7 single crystals

The TL glow curve of X-ray irradiated pure and Cu-doped Li₂B₄O₇ shows that the most intense TL peak is at 160°C. In the present work the characteristics of the TL and PTTL glow curves from gamma irradiated pure Li₂B₄O₇ single crystal samples (prepared by Mitui Kinzoku Kougyo, Japan) have been studied. The samples were irradiated with different gamma doses (from 0.5 up to 500 Gy) using a ⁶⁰Co gamma ray source at a dose rate of 78 Gy h⁻¹. The TL glow curve shows three intense peaks (at 160°C, 260 and 305°C) and three weak ones (at 110, 140 and 220°C). The most intense TL peak is at 160°C, which agrees with the TL glow curve from X-ray irradiated samples [Kutomi Y. and Tomita A. (1990) TSEE and TL of Li₂B₄O₇:Cu single crystals. Radiat. Prot. Dosim. 33, 347–350]. The 305°C peak in gamma irradiated samples also appears to be very intense, which indicates its possible use in high-dose high-temperature dosimetry. Further, the characteristics of the PTTL glow curve have been studied as a function of ultraviolet exposure and number of repeated PTTL cycles.     

Thermoluminescence of natural and synthetic diopside

Diopside, a natural silicate mineral of formula CaMgSi₂O₆, has been investigated concerning its thermoluminescence (TL) and electron paramagnetic resonance (EPR) properties. Glow curves and TL vs. γ-dose were obtained irradiating natural samples to additional dose varying from 50 to 10,000 Gy. Except for a 410 °C peak found in the Al-doped artificial diopside, all the other peaks grow linearly with radiation dose, but saturate beyond 1 kGy. To investigate high-temperature effect before irradiation, measurements of TL intensity in samples annealed at 500–900 °C and then irradiated to 1 kGy γ-dose were carried out. Also the TL emission spectrum has been obtained. To compare with natural diopside, a synthetic pure polycrystal was produced and further those doped with iron, aluminum and manganese were also produced.     

Optical and dosimetric properties of variously doped SrF2 crystals

Optical properties and irradiation effects of Nd³⁺-, Pr³⁺-, Tb³⁺- and Tm³⁺-doped SrF₂ crystals and their possible application to solid-state dosimetry were studied and compared to those induced in pure SrF₂ crystals. Optical absorption, thermoluminescence (TL), X- and light-induced luminescence (XL and PL) as well as optically stimulated luminescence and phototransferred TL (OSL and PTTL) were measured in the various samples. Special attention was given to effects of monochromatic vacuum ultraviolet (VUV) radiation. TL was excited in the pure and doped samples by X and β rays as well as by VUV radiation. TL peaks appeared after VUV irradiation at the same temperatures and with the same thermal activation energies as after X or β irradiation, indicating that they are due to the same processes. The VUV excitation spectra showed two maxima at about 145 and 130 nm. Comparison of the TL sensitivities of the various TL materials, showed that the sensitivity of SrF₂:Pr³⁺ was by more than an order of magnitude higher than that of the known LiF:Mg,Ti (TLD-100) phosphor. The sensitivity of pure and of the Nd, and Tb-doped SrF₂ were by a factor of 2–4 higher than that of the TLD-100 and that of SrF₂:Tm was slightly lower. The main emission bands of SrF₂:Pr³⁺ are located in a convenient spectral region between 460 and 640 nm, where most of the standard photomultipliers are sensitive. The dose dependence of the 460 K TL peak in SrF₂:Pr³⁺ is nearly linear in a wide range up to above 27 000 Gy.     

不同退火温度的Al_2O_3:C薄膜热释光和光释光性能

α-Al_2O_3:C晶体的热释光和光释光性能优越,但其制备要求高,需高温和高还原气氛.与α-Al_2O_3:C晶体性能接近的α-Al_2O_3:C陶瓷,热释光峰不单一.本文采用两次阳极氧化法在0.5 mol/L的草酸溶液中5℃恒温制备高度均匀有序的多孔Al_2O_3:C薄膜,主要研究不同退火温度对其热释光和光释光特性的影响.结果表明,经不同温度退火后的Al_2O_3:C薄膜均为非晶结构;不同退火温度的Al_2O_3:C薄膜热释光的主发光峰约在310℃左右,符合通用级动力学模型.600℃退火后的Al_2O_3:C薄膜热释光灵敏度最强,其热释光剂量曲线在1-10 Gy范围内具有很好的线性响应,在剂量10-120 Gy范围内出现超线性响应;在相同的辐照剂量下,随着退火温度的升高(≤600℃)光释光的初始发光强度逐渐增强.不同退火温度的Al_2O_3:C薄膜光释光衰减曲线都呈典型的指数衰减且快衰减速率相比α-Al_2O_3:C晶体显著加快.600℃退火后的Al_2O_3:C薄膜光释光灵敏度最强,其光释光剂量响应曲线在1-200 Gy整体上都具有很好的剂量线性关系.与热释光相比,Al_2O_3:C薄膜的光释光具有更宽的线性剂量响应范围.此研究为Al_2O_3:C薄膜作为光释光辐射剂量材料做出了有益的探索.     

Defect versus nanocrystal luminescence emitted from room temperature and hot-implanted SiO2 layers

Silicon nanocrystals have been synthesized in SiO₂ matrix using Si ion implantation. Si ions were implanted into 300-nm-thick SiO₂ films grown on crystalline Si at energies of 30–55 keV, and with doses of 5×10¹⁵, 3×10¹⁶, and 1×10¹⁷ cm⁻². Implanted samples were subsequently annealed in an N₂ ambient at 500–1100°C during various periods. Photoluminescence spectra for the sample implanted with 1×10¹⁷ cm⁻² at 55 keV show that red luminescence (750 nm) related to Si-nanocrystals clearly increases with annealing temperature and time in intensity, and that weak orange luminescence (600 nm) is observed after annealing at low temperatures of 500°C and 800°C. The luminescence around 600 nm becomes very intense when a thin SiO₂ sample is implanted at a substrate temperature of 400°C with an energy of 30 keV and a low dose of 5×10¹⁵ cm⁻². It vanishes after annealing at 800°C for 30 min. We conclude that this luminescence observed around 600 nm is caused by some radiative defects formed in Si-implanted SiO₂.     

2018年7期 电子期刊

采用自蔓延燃烧法制备了不同镨掺杂浓度的12CaO·7Al₂O₃：Pr³⁺（C12A7：Pr³⁺） X射线影像存储荧光粉。在232 nm激发下,发现Pr³⁺掺杂摩尔分数为0.3%的荧光粉位于486 nm的蓝光发射峰呈现最大的发光强度。对C12A7：0.3% Pr³⁺样品进行真空热处理后,C12A7笼中的O^2-基团数量减少,同时类F⁺色心的空笼子的数量增多,导致陷阱数目增加和光激励发光强度增大。热释发光实验表明：C12A7：0.3% Pr³⁺样品中存在两个深陷阱,陷阱深度分别约为0.69 eV和0.80 eV;经过真空热处理后的C12A7：0.3% Pr³⁺荧光粉,陷阱深度变深,陷阱数目增多,光存储性能变好。当吸收的X射线剂量为5.2 Gy时,可以实现分辨率较高的X射线成像。实验结果表明,镨掺杂C12A7荧光粉在计算机X射线摄影领域有潜在的应用前景。     

Extending the time range of luminescence dating using red TL (RTL) from volcanic quartz

The potential of red thermoluminescence (RTL) emission from quartz, as a dosimeter for baked sediments and volcanic deposits, has received some attention over the past decade. While there have been some important observations relating to signal stability, saturation characteristics and emission wavebands, there has not been a systematic analysis of RTL properties of older (i.e., >1 Ma), quartz-bearing known age volcanic deposits. We have undertaken such an analysis using independently-dated silicic volcanic deposits from New Zealand, ranging in age from 300 ka through to 1.6 Ma. We observed a complex RTL emission in most volcanic quartzes, which consists of a number of discrete high temperature (i.e, >220°C) TL peaks. Isothermal analysis indicates a stable dating trap (E=2.03 eV; S=4.20×10¹⁵) which is stable at ambient (c. 20°C) temperatures for >10⁹ a. We confirm the slow onset of saturation with dose, and the limited extent of sensitivity changes due to dosing and TL readout. As such, there is much potential for exploiting the dosimeter in dating studies and we present the results from a modified single aliquot regenerative (SAR) procedures which indicate that there is a good agreement between RTL dating and other methods over time scales 10⁵–10⁶ a. This paper presents a summary of the most important related results of our findings and outlines the configuration of photomultiplier and filter combinations which maximizes RTL detection for temperatures up to 500°C.     

TL response of a natural fluorite

A batch of a naturally occurring fluorite (CaF₂) from the Middle Benue Valley region of Nigeria has been studied in some detail for its thermoluminescence (TL) properties. TL glow peaks are observed at 119, 144 and 224°C at a heating rate of 10°C s⁻¹. The TL response is observed to increase with increasing dose, as expected, over the dose range examined. Variations are observed in the decay curves of the various glow peaks with storage at room temperature. While the lower temperature peaks are observed to decay, enhancement of the TL signal is observed for the 224°C glow peak when stored for four weeks. A low-level radioactivity measurement showed no evidence of self-irradiation from naturally occurring radionuclides. UV exposure was suppressed by storage in a black sealed container to exclude sunlight contribution to the observed TL response. A scheme involving the formation of large defect complexes, from smaller ones, during storage, as possible route leading to loss of signal in low temperature glow peaks and a corresponding enhancement at higher temperature, is suggested.     

退火对Pb辐照Al2O3单晶发光特性的影响

研究了230MeV的²⁰⁸Pb²⁷⁺辐照Al₂O₃样品及随后在600,900,1100K高温条件下退火后的光致发光特性。从辐照样品的测试结果可以清楚地看到在波长为390,450nm处出现了强的发光峰。辐照量为1×10¹³ions/cm²时,样品的发光峰最强。经过600K退火2h后测试结果显示,380nm发光峰剧烈增强,而其他发光峰显示不明显。在900K退火条件下,380nm的发光峰开始减弱,而在360,510nm出现了明显的发光峰,至到1100K退火完毕后380nm的发光峰完全消失,而360,510nm的发光峰相对增强。从被辐照样品的FTIR谱中看到,波数在460~510cm^-1间的吸收是振动模式,经过离子辐照后,吸收带展宽,随着辐照量的增大,Al₂O₃振动吸收峰消失,说明Al₂O₃振动模式被完全破坏。1000~1300cm^-1之间为Al—O—Al桥氧的伸缩振动模式,辐照后吸收带向高波数方向移动,说明其振动模式受到影响。辐照剂量较小的样品,损伤程度相对较低,经退火晶化后,振动模式基本恢复到单晶状态;辐照剂量较高的样品,损伤程度大,退火处理后表面变得较粗糙,振动模式并未出现,说明结构破坏严重。     

LiMgPO_4:Tm,Tb的热释光和光释光陷阱参数

采用高温固相法合成了LiMgPO_4:Tm,Tb粉末样品,测定了热释光陷阱参数激发能E和频率因子s.用脉冲退火和多次退火方法研究了其光释光陷阱参数E和s,并与用多速法得到的热释光的结果进行了比较.对不同β射线剂量照射的样品发光曲线的研究表明,300°C高温峰属于一级动力学发光峰.通过对热释光和光释光陷阱的相关性研究表明,经200°C预热的热释光信号(对应于300°C高温峰)和光释光信号很有可能来自于同一深度的陷阱.     

The effects of hydrogen dose and thermal treatment on the formation of microsplits in hydrogen implanted GaAs

Transmission electron microscopy has been used to study the effect of thermal treatment on the formation of microsplits and damage rafts in hydrogen implanted (1 × 10¹⁶ and 5 × 10¹⁶ H⁺ cm^-2) and annealed (700 and 800°C) GaAs. The results show that microsplit and damage raft formation in implanted samples may be prevented if the samples are first given a pre-anneal heat treatment for 15 minute intervals at 300, 350, 400 and 450°C, during which the hydrogen concentration is reduced without allowing vacancy coalescence to take place.     

Phototransferred Thermoluminescence of Dosimetric α-Al<Subscript>2</Subscript>O<Subscript>3</Subscript> Crystals Irradiated by a Pulsed Electron Beam

The thermoluminescence (TL) of deep traps of anion-defective alumina monocrystals irradiated by a high-dose (more than 1 kGy) pulsed electron beam (130 keV) is studied. The deep traps in the studied material are classified according to the TL temperature range. It is demonstrated that the phototransferred thermoluminescence (PTTL) in the temperature range of the main TL peak is induced by optical charge migration from deep traps that are emptied at 400–470 and 470–600°C. An anomalous PTTL enhancement in crystals subjected to stepped annealing in the 350–400°C interval is observed. It is demonstrated that this effect may be caused by competing processes of charge transfer that involve deep traps corresponding to the TL peak at 390°C. The applicability of PTTL in the dosimetry of high-dose (1–50 kGy) pulsed electron beams is established.     

The effect of boron ion implantation and annealing on the microstructure and electrical characteristics of the diamond films

Diamond films were doped by boron ion-implantation with the energy of 120 keV. The implantation dose ranged from 10¹⁴ to 10¹⁷ cm⁻². After the implantation, the diamond films were annealed at different temperatures (600–750°C) for different times (2–15 min). Scanning Electronic Microscope, Raman and Secondary Ion Mass-spectrum were used to investigate the effect of boron ion implantation and annealing on the microstructure of the diamond films. The electrical resistivities of the diamond films were also measured. It was found that the best dose of boron ion-implantation into the diamond film was around 10¹⁶ cm⁻². The appropriate annealing temperature and time was 700°C and 2–5 min, respectively. After implantation, the resistivities were reduced to 0.1 Ω cm (almost nine orders lower than the unimplanted diamond films). These results show that boron ion implantation can be an effective way to fabricate P-type diamond films.     

Electrical characterization of argon-ion sputtered n-GaAs

Epitaxially grown n-type GaAs was sputtered with 0.5 keV Ar ions at doses of 10¹² and 10¹⁵ ions/cm². The sputter-induced defects in the GaAs were characterized using deep-level transient spectroscopy (DLTS) and the effect of these defects on the characteristics of Au Schottky barrier diodes (SBD's) fabricated on the sputtered GaAs was evaluated by current-voltage measurements. It was found that the barrier height of the SBD's decreased with ion dose from 0.97 eV for unsputtered diodes to 0.48 eV after sputtering at a dose of 10¹⁵/cm². DLTS showed the presence of a multitude of sputter-induced defects at and near the GaAs surface. The defects formed during the initial stages of sputtering had the same properties as some of the primary defects introduced during electron and proton irradiation of GaAs. Isochronal annealing at temperatures of up to 350°C showed that although some defects were removed by annealing, others appeared.     

低温燃烧合成法制备的氧化铝陶瓷粉体的发光特性

α-Al₂O₃∶C单晶具有优良的热释光特性,被用做热释光剂量计,但α-Al₂O₃∶C晶体剂量计的形状不易加工,生产成本高且碳在晶体中难以掺杂均匀。采用低温燃烧合成法以无水乙醇为溶剂,尿素为染料,硝酸铝为反应物制备少团簇、分散均匀的片状α-Al₂O₃∶C陶瓷粉体。探讨不同点火温度和不同退火温度对其光致发光特性的影响,不同退火温度对热释光特性的影响以及热释光与辐射剂量(90Sr β)的关系。通过分析α-Al₂O₃∶C陶瓷粉体的光致发光光谱得出：α-Al₂O₃∶C陶瓷粉体的发射波长在395 nm附近,点火温度T≤800℃时,点火温度为500 ℃制备的α-Al₂O₃∶C陶瓷粉体的光致发光强度最强;在相同点火温度T=500 ℃下,经不同温度退火制备α-Al₂O₃∶C陶瓷粉体,点火温度为500 ℃制备的α-Al₂O₃∶C陶瓷粉体经1 000 ℃退火后光致发光强度最强。通过分析α-Al₂O₃∶C陶瓷粉体的热释光曲线得出：退火后的α-Al₂O₃∶C陶瓷粉体在200 ℃左右的热释光峰值占主导,900 ℃退火的α-Al₂O₃∶C陶瓷粉体在200 ℃附近的热释光峰值最强;通过峰高法对900 ℃高温退火处理后的α-Al₂O₃∶C陶瓷粉体位于200 ℃左右的热释光峰做剂量响应曲线,可以看出,在1～50 Gy剂量范围内具有良好的热释光剂量线性响应关系,在50～200 Gy剂量范围内出现超线性响应关系。与α-Al₂O₃∶C晶体(1～10 Gy)和多孔Al₂O₃∶C薄膜(1～10 Gy)相比,α-Al₂O₃∶C陶瓷粉体的线性剂量响应范围明显扩大。此研究可为提高氧化铝陶瓷粉体的热释光性能提供思路。     

Effects of type of radiation on glow curve and thermoluminescence emission spectrum of CaF2:Tm

Thermoluminescence emission spectra of CaF₂:Tm (TLD-300) samples irradiated with 48 keV X-rays ⁶⁰Co gamma rays, 4.5 MeV alpha particles and 15 MeV neutrons were measured in the 300–650 K temperature region. Seven emission bands were observed of which the one in the infrared (at 803 nm) is very intense. The emission bands can be assigned to ¹D, ¹G, ³F and ³H levels characteristic for Tm³⁺ de-excitation in a cubic field. All observed lines in the spectrum are due to 4f-4f transitions. The spectra undergo remarkable changes in intensity when the temperature is raised from room temperature up to 350°C, while the number of the emission bands remains constant. The glow curve structure is both dependent on emission wavelength and the type of radiation. Evidence has been found that the trapping structures responsible for glow peaks 2 and 3 alter under the influence of high LET () radiation. For glow peaks 4–6 the filling of the traps alters with the type of radiation. The observations can be explained assuming a TL process involving several hole trapping centres but with only one luminescent centre (Tm³⁺) active at all temperatures.     

Comparison of blue and red TL from quartz

Following a suggestion by Scholefield and Prescott that blue and red emissions in quartz may involve the same electron traps, we have made a detailed study of blue and red TL glow peaks in some Australian sedimentary quartz samples (Scholefield, R.B., Prescott, J.R., 1999. The red thermoluminescence of quartz: 3-D spectral measurements. Radiat. Meas. 30, pp. 83–95). Allowing for thermal quenching of the blue TL, the Rapidly Bleaching Peak (at 325°C for a ramp rate of 20 K s⁻¹) and the low temperature peaks at 140–220°C appear to be identical in the blue and red. We conclude that the electron traps are the same, but that the blue and red luminescence centers probably do not occur in the same grains. On present evidence we cannot determine whether or not the Slowly Bleaching Peak (at 375°C for 20 K s⁻¹) involves the same traps in the blue as in the red. As did Scholefield and Prescott, we find no evidence of a red peak at 100°C.     

Study of the 110°C TL peak sensitivity in optical dating of quartz

As the 110°C TL emission in quartz uses the same luminescence centers as the OSL emission, the 110°C TL signal from a test dose may be used to monitor the OSL sensitivity change. It is thus important to study the relationship between the 110°C TL peak and the OSL sensitivity in studies related to optical dating from quartz. We have conducted a series of experiments using sedimentary quartz, where the annealing temperatures were varied between 260 and 1000°C before the measurement of OSL and 110°C TL sensitivities. Another series of experiments on two sedimentary quartz samples investigated the 110°C TL peak and OSL dose-dependent sensitivity change after different annealing temperatures. In these experiments, the 110°C TL and OSL signals from the test dose are shown to have similar sensitization characteristics: the 110°C TL sensitivity change is proportional to the OSL sensitivity change if the annealing temperature is lower than 500°C. It is concluded that the 110°C TL signal can be used to correct the OSL sensitivity change in the single-aliquot additive-dose protocol.     

Luminescence and circularly polarized luminescence of macrocyclic Eu(III) and Tb(III) complexes embedded in xerogel and sol–gel SiO2 glasses

Luminescence, time-resolved luminescence, circularly polarized luminescence (CPL) and decay profiles of Ln(III)(15-crownether-5) (Ln=Ce, Sm, Eu, Tb) and Tb(III)-(R),(S)-cyclen derivative complexes doped in xerogel and sol–gel silica glasses are measured at temperatures down to 10 K to characterize luminescence properties and the electronic structure in the excited states. Luminescence spectral profiles and calculation of crystal field parameters (B₀⁽²⁾,B₂⁽²⁾) in the ⁵D₀→⁷F_J(J=1,2) transition give evidence of the fact that the pentagonal and planar structure of Eu(III) (15-crownether-5) does hold in xerogel and sol–gel glasses prepared at temperatures below 100°C. As annealing temperatures are increased from 80°C to 750°C, Eu(III) complexes in sol–gel glasses are found to decompose gradually to SiO₂:Eu³⁺. Tb(III)-(R) and (S)-cyclen derivative complexes in xerogel reveal at room temperature and 10 K sharp CPL spectra with luminescence dissymmetry factors g_lum=−0.1 and 0.1, respectively. These complexes doped in sol–gel glasses represent luminescence characteristics of rare earth ions encapsulated in the nano-porous host.     

Buffers for high temperature superconductor coatings. Low temperature growth of CeO2 films by metal–organic chemical vapor deposition and their implementation as buffers

Smooth, epitaxial cerium dioxide thin films have been grown in-situ in the 450–650°C temperature range on (001) yttria-stabilized zirconia (YSZ) substrates by metal–organic chemical vapor deposition (MOCVD) using a new fluorine-free liquid Ce precursor. As assessed by X-ray diffraction, transmission electron microscopy (TEM), and high-resolution electron microscopy (HREM), the epitaxial films exhibit a columnar microstructure with atomically abrupt film-substrate interfaces and with only minor bending of the crystal plane parallel to the substrate surface near the interface and at the column boundaries. With fixed precursor temperature and gas flow rate, the CeO₂ growth rate decreases from 10 Å/min at 450°C to 6.5 Å/min at 540°C. The root-mean-square roughness of the films also decreases from 15.5 Å at 450°C to 4.3 Å at 540°C. High-quality, epitaxial YBa₂C₃O_7−x films have been successfully deposited on these MOCVD-derived CeO₂ films grown at temperatures as low as 540°C. They exhibit T_c=86.5 K and J_c=1.08×10⁶ A/cm² at 77.4 K.