Natural luminescence and anomalous fading in K-feldspar

This study investigated the relationship between the natural luminescence intensity, the amplitude of anomalous fading and the apparent IRSL age of a suite of feldspar single grains. Correlating natural luminescence with fading may simplify the identification of weakly to non-fading feldspars grains in sediments. In our single grain experiments, the mean fading corrected IRSL age obtained from a small population of bright grains is close to the expected depositional age of the sediment investigated. It is proposed that in dating programs, more attention should be given to bright feldspar grains as they are the most stable grains in the population.     

Sources of overdispersion in a K-rich feldspar sample from north-central India: Insights from De,K content and IRSL age distributions for individual grains

Luminescence dating of individual sand-sized grains of quartz is a well-established technique in Quaternary geochronology, but the most ubiquitous mineral on the surface of the Earth—feldspar—has received much less attention at the single-grain level. In this study, we estimated single-grain equivalent dose values and infrared stimulated luminescence (IRSL) ages for K-rich feldspar (KF) grains from a fluvial sample underlying Youngest Toba Tuff (YTT) deposits in north-central India, and compared these ages (corrected for anomalous fading) with those obtained from individual grains of quartz from the same sample. Both minerals have broadly similar single-grain age distributions, but both are greatly overdispersed and most grains have ages substantially younger than the expected age of the YTT deposit (～74 ka). Almost half (45%) of KF grains used for age calculation have fading rates statistically consistent with zero, but the age distribution of these grains is as dispersed as that of the entire population. We obtained a similar distribution of ages calculated for 51 grains using their individually measured internal K contents, which exhibited only minor grain-to-grain variation. Given the lack of dependency of single-grain ages on the measured fading rates and internal K contents, and the overall adequacy of bleaching of grains collected from a sandbar in the modern river channel, we consider the spread in ages is most likely due to mixing, at the time of deposition and after the YTT event, of potentially well-bleached fluvially-transported sediments with older grains derived from slumping of riverbank deposits. Some spread may also be due to natural variations in the IRSL properties of individual KF grains.     

Na-rich feldspar as a luminescence dosimeter in infrared stimulated luminescence (IRSL) dating

One of the challenges in dating rock surfaces is the choice of the luminescence mineral. Although quartz is the preferred dosimeter in sediment dating, it is often not sufficiently sensitive when extracted from solid rocks. The intensity of signals from feldspars tends to be much less dependent on geological origin and erosion history, but the dosimetry of K-rich feldspar grains extracted from rocks is complicated because the internal dose rate is very dependent on the original feldspar grain size. The in situ grain size information is lost during the crushing process used to separate the grains for measurement. This latter problem does not apply to Na-rich feldspar because of the absence of internal radioactivity.The potential application of Na-rich feldspar as a luminescence dosimeter for the IRSL dating of rock surfaces is investigated using a variety of sediment samples from different geological settings for which independent age control is available. The blue and yellow luminescence emissions are measured for IR stimulation at 50 °C (IR₅₀), and post-IR IR stimulation at 290 °C (pIRIR₂₉₀). Thermal stability experiments imply that the corresponding signals in both emissions have comparable thermal stabilities and that all signals have similar recombination kinetics and are thermally stable over geological timescales. The IR₅₀ doses measured using blue and yellow emissions are similar to or lower than quartz doses while pIRIR₂₉₀ blue doses are higher than those from yellow emission and quartz doses. The fading rates measured for the IR₅₀ signals are ∼3%/decade larger than those measured for the pIRIR₂₉₀ signals in both yellow and blue emissions. Furthermore the average fading rates of both yellow signals are ∼3%/decade higher than the corresponding fading rates of the blue signals. However, there is no detectable correlation between fading rates and the measured D_e values. The residual doses measured from the laboratory-bleached samples and a modern analogue suggest that the IR₅₀ signals in both blue and yellow emissions bleach to the same degree, as do the corresponding pIRIR₂₉₀ signals, and that there is no significant naturally-unbleachable residual dose observed using these signals. Neither anomalous fading nor incomplete bleaching explains the observed dose discrepancy between the two emissions. Eight uncorrected and fading-corrected ages are calculated for each sample based on all four signals, using the dose rate relevant to Na-rich feldspar extracts (i.e. ∼3% K). The IR₅₀ and pIRIR₂₉₀ blue ages were also calculated assuming a dose rate based on 12.5% internal K (i.e. assuming that the blue signals were mainly derived from contamination by K-rich feldspar). The latter pIRIR₂₉₀ blue ages are in agreement with the expected age control, raising the possibility that this signal originates mainly from K-rich feldspar contamination in our Na-rich fractions, and thus is not so useful in the luminescence dating of rock surfaces. On the other hand, the pIRIR₂₉₀ fading-corrected ages based on the yellow emission are consistent with the independent age controls; higher preheat and stimulation temperatures may result in more stable yellow signals from Na-rich feldspar extracts from rocks, and so reduce the size of the fading correction. We conclude that, because this signal avoids the dosimetry difficulties of K-rich feldspar extracts, it has considerable potential in the IRSL dating of rock surfaces.     

Red luminescence from potassium feldspar for dating applications: a study of some properties relevant for dating

Aspects of the red thermoluminescence (RTL) and IR (833±5 nm) stimulated red (λ_emission=600–750 nm) luminescence (orange-red IRSL) of potassium feldspar from different origins are described. Anomalous fading of RTL (300–500°C) from a selection of potassium feldspar samples was tested. High temperature RTL (300–450°C) exhibits less anomalous fading in comparison to UV luminescence, for the samples under study. The result supports the contention of Zink and Visocekas (1997) that the red TL emission from feldspar does not fade. It was found that RTL is bleachable due to IR exposure, and the relationship between RTL lost and orange-red IRSL produced is linear. It is shown that around one third of the trapped charge responsible for the orange-red IRSL signal gives rise to an RTL signal, indicating that some traps and luminescence centres are shared for RTL and orange-red IRSL.

Specific characteristics of orange-red IRSL from feldspar were identified. It was found that the orange-red IRSL decay curve is bleachable by IR and daylight and can be described by the sum of three exponential components. Orange-red IRSL fading was tested. Short-term storage tests (up to 2 weeks) showed no fading. Longer-term (ca. months) storage of orange-red IRSL do in fact indicate fading, though at levels considerably lower than for the UV emission. The contradictory result is possibly due to the detection wavelength. As such, it is highly likely that the long-term fading experiment is strongly influenced by the feldspar emission centred at ca. 570 nm, which exhibits anomalous fading, while the short-term fading experiment is more greatly influenced by the far red emission centred at ca. 710 nm that in comparison to UV emission shows no or less fading.     

Spectral study on feldspar thermoluminescence process

Feldspar thermoluminescence fading phenomena were investigated here by using newly-constructed thermoluminescence spectrometer on the basis of charge-coupled detector, and thereafter the discussion and explanation on feldspar TL fading mechanism were presented. The experimental results show that the fading rate of feldspar TL depends on both wavelength and stimulated temperature, and normally the feldspar TL in every region of wavelength and temperature shows different traits, namely the low temperature TL (170°–190°) fading at the rate of logarithmic function and furthermore the TL of different wavelengths fading at approximately the same rate on the condition of 160° preheating. While the medium and high temperature TLs (290°–400°) do not show much thermal fading, their fading rate at room temperature invariably correlates well with their wavelength, namely the longer TL wavelength, the slower TL fading rate. The thermal instability of traps and the quantum-mechanical tunneling effects can explain the above fading phenomena respectively. It is recognized that feldspar TL fading depends on its wavelength, and furthermore new aspects of the solid thermoluminescence process can be displayed by the combination of three-dimensional TL spectral analysis and thermal fading or anomalous fading of TL for feldspar. Supported by the National Natural Science Foundation of China (Grant No. 40534019) and the Knowledge Innovation Program of the Chinese Academy of Sciences (Grant No. GIGCX3-07-10)     

Detailed study of a thermoluminescent mineral exhibiting anomalous fading

Anomalous fading, the unexpected loss of charge carriers responsible for high temperature thermoluminescence, has been shown to affect some minerals that are found in samples proposed for archaeological and geological thermoluminescence (TL) dating studies. This paper describes detailed studies of the phenomenon in one feldspar sample. Three possible explanations are considered and further experiments are proposed to distinguish between them. The implications of anomalous fading for TL dating are assessed and some ways of circumventing its ill-effects are suggested.     

The single-aliquot regenerative-dose (SAR) protocol applied to coarse-grain feldspar

The application of the single-aliquot regenerative-dose (SAR) protocol to equivalent dose determination in coarse-grain feldspar is investigated. An outline of the protocol is presented, and basic tests of its performance are discussed. It is shown that the method is robust and yields results similar to those obtained with a single-aliquot additive-dose (SAAD) procedure. The use of the SAR procedure for fading tests is also discussed. We conclude that the SAR protocol for coarse-grain feldspar yields several advantages over previously used multiple-aliquot and single-aliquot methods. The method is fast and precise, the equivalent dose is obtained by interpolation, and the method corrects for sensitivity changes. The luminescence age obtained by SAR and additive-dose dating of the coarse-grain feldspar separates used in this study do, however, underestimate the independently estimated geological age of the samples.     

Time-resolved infrared stimulated luminescence signals in feldspars: Analysis based on exponential and stretched exponential functions

Time-resolved infrared-stimulated luminescence (TR-IRSL) signals from feldspar samples have been the subject of several recent experimental studies. These signals are of importance in the field of luminescence dating, since they exhibit smaller fading effects than the commonly employed continuous-wave infrared signals (CW-IRSL). This paper presents a semi-empirical analysis of TR-IRSL data from feldspar samples, by using a linear combination of exponential and stretched exponential (SE) functions. The best possible estimates of the five parameters in this semi-empirical approach are obtained using five popular commercially available software packages, and by employing a variety of global optimization techniques. The results from all types of software and from the different fitting algorithms were found to be in close agreement with each other, indicating that a global optimum solution has likely been reached during the fitting process. Four complete sets of TR-IRSL data on well-characterized natural feldspars were fitted by using such a linear combination of exponential and SE functions. The dependence of the extracted fitting parameters on the stimulation temperature is discussed within the context of a recently proposed model of luminescence processes in feldspar. Three of the four feldspar samples studied in this paper are K-rich, and these exhibited different behavior at higher stimulation temperatures, than the fourth sample which was a Na-rich feldspar. The new method of analysis proposed in this paper can help isolate mathematically the more thermally stable components, and hence could lead to better dating applications in these materials.     

Infrared (IR) stimulated luminescence from modern bricks in retrospective dosimetry applications

It has frequently been observed that certain roof tiles and bricks, especially from relatively modern European buildings, do not contain enough quartz grains in a suitable grain size range to permit dose reconstruction using thermoluminescence (TL) or optically stimulated luminescence (OSL) methods. In this paper the feasibility of using infrared-stimulated luminescence (IRSL) on the feldspar fraction of such bricks and tiles has been investigated. Appropriate preheating treatments were employed in order to select the most stable signals, and procedures were developed to enhance the signal to noise ratio. The possible effect of anomalous fading under application of these procedures was tested. In the dose range above 100 mGy, it has been demonstrated that using IRSL on the feldspar fraction of such material provides a feasible alternative to the use of green-light-stimulated luminescence (GLSL) on the quartz fraction, for the purposes of retrospective dosimetry. Furthermore, since the use of IRSL as described in this paper involves the measurement of polymineral fine grain fractions of bricks, a technique for the calibration of the built-in β source against the γ source in Secondary Standard Dosimetry facilities for routine use of the technique is described.     

Application of pulsed OSL to polymineral fine-grained samples

Pulsed OSL is applied to nine fine-grained sediment samples from Sichuan province, China, using stimulating pulses of 10 μs on and 240 μs off, with an infrared exposure prior to each OSL measurement. Comparison of fading rates between pulsed and non-pulsed signals, the latter also obtained with a preceding IR exposure, shows that fading is significant for mainly the non-pulsed signals. Presence of a pulsed IRSL and the magnitudes of b-value to correct for lower alpha efficiency suggest that pulsing does not fully remove a significant feldspar signal, only a fading component. Comparison with ages of quartz extracts shows that pulsed OSL ages are consistent, while CW-OSL ages are slightly older and CW-IRSL ages are much older. The older ages suggest a less well-bleached feldspar component.     

Dynamics of microcracks and time dependences of surface deformation of a heterogeneous body (granite) under an impact

The dynamics of fractoluminescence flashes and the time dependences of surface deformation of granite with different sizes of feldspar grains under an impact on samples by a metal pin have been studied with a 10 ns resolution. A band at ??1.9 eV has been observed in the fractoluminescence spectra, which means that, under the influence of mechanical stresses, Si-O-Si bonds are broken and ?? SiO^?? free radicals are formed. The fractoluminescence has the form of flashes with a duration of ??10 ns. It has been assumed that each of them corresponds to the nucleation of a microcrack. From the flash intensities and the elastic wave velocity, the linear size of microcracks has been estimated to be from ??8 to 30 ??m. Microcracks are mainly generated during passage of a deformation wave through feldspar grains. An impact causes the appearance of eigenvibrations of the entire sample, and cracking of grains gives rise to eigenvibrations of grains.     

Monitoring anomalous fading of TL of feldspars by using far-red emission as a gauge

TL dating of feldspars of volcanic origin is thwarted by anomalous fading of its emission in the usual spectral range from UV to red, though in the far-red range it has been shown to be stable. A new method of evaluation of this anomalous fading is proposed. The comparison is no longer made directly between total TL emissions after different storage times. Instead, TL is first measured in two spectral ranges simultaneously, the ‘blue’ one, usually monitored for fading, and the far-red one. Secondly, at every temperature the ratio of ‘blue’ to far-red, named B_ir, is computed. Thirdly, to monitor anomalous fading, these ratios are compared between different TLs. When fading shows, values of B_ir are observed to decrease during storage, according to the logarithmic law, down to very low values. A temperature dependance of anomalous fading is firmly established.     

周口店花岗闪长岩中斜长石晶体化学及谱学特征研究

前人研究多集中于碱性长石等其他长石系列,对斜长石的研究较少。在野外地质工作的基础上,采用电子探针仪、X光粉晶衍射仪、红外光谱仪和拉曼光谱仪对周口店花岗闪长岩中自然产出的斜长石进行了谱学特征和化学成分分析。电子探针分析获得该地斜长石的化学成分,端元组分在Ab_(85.21)Or_(0.18)An_(9.11)到Ab_(90.06)Or_(3.00)An_(13.27)之间;斜长石的X光粉晶衍射特征说明样品组成为较为纯净的钠长石,根据粉晶衍射峰及其衍射强度计算得出了样品晶胞参数;采用红外光谱和拉曼光谱分析了斜长石的谱学特征并对特征吸收谱带和特征峰进行了归属。在OH-红外吸收区(3 000～3 800 cm-1)出现了由OH的伸缩振动导致的特征吸收谱带: 3 200, 3 310,3 420和3 615 cm-1,表明研究区的钠长石普遍含有结构水,以OH-的形式存在。在以上分析的基础上对此种长石的晶体化学和结构特征进行了归纳总结。     

Investigating the contribution of recuperated TL to post-IR IRSL signals in a perthitic feldspar

Using a museum specimen of perthitic feldspar, the characteristics of post-IR IRSL production at 200 °C after different prior IR bleaching at 100 °C were investigated. It was found that the post-IR IRSL signal had an isothermal TL contribution that was unexpected following a previous preheat at 320 °C; this is the result of isothermal decay of recuperated TL peaks resulting from photo-transfer that occurred when the previous IRSL signal was measured at a lower temperature. The isothermal TL contribution to the post-IR IRSL signal depends on prior IR bleaching conditions. Since the recuperated TL signal comes from photo-transfer during IRSL production, this signal should also suffer from anomalous fading. Thus, it is suggested that this isothermal TL contribution to the measured post-IR IRSL is removed by the inclusion of an additional step, a cut-heat to 300 °C, in the post-IR IRSL dating protocol.     

Nanosecond dynamics of destruction of an inhomogeneous solid (granite) induced by an impact on its surface

Dynamics of microcrack formation and deformation of a granite-sample surface after a striker impact have been studied with a time resolution of 2 ns. The impact excites the sample’s natural vibrations that lead to formation of clusters of microcracks with linear dimensions of ~2 to 10 μm in feldspar grains. The formation of microcracks, in turn, excites natural vibrations of the grains.     

Apparent anomalous fading of thermoluminescence associated with competition with radiationless transitions

Anomalous fading of thermoluminescence (TL) is the effect of a fading which is significantly faster than what is warranted by the trapping parameters which are evaluated from the features of the TL peak in question. A previous work suggested that in certain cases, apparent anomalous fading may be a normal fading in disguise. The idea was that, at least in some cases, radiationless transitions into competing recombination centers may yield a very narrow peak which, while using either the curve fit technique or the different peak shape method will result in very high values of effective activation energy E and frequency factor s which, in turn, will yield an apparent life-time orders of magnitude higher than the real one. The question has been raised whether this anomaly is observable only when the peak shape methods are utilized and in particular, can the same effect occur when the broadly used initial-rise method is applied. It is demonstrated in this work that under similar circumstances of competition, very high effective values of E and s are evaluated which result in very high life-times when the activation energy is evaluated by the initial-rise method. Thus, the explanation of apparent anomalous fading as being a normal decay in disguise, is extended to cases in which the initial-rise method is utilized for the parameter evaluation.     

Natural IRSL intensities and apparent luminescence ages of single feldspar grains extracted from partially bleached sediments

The single aliquot technique has been applied to single grains of K-feldspar extracted from a well-dated late-glacial marine sediment sample for which standard luminescence dating yielded ages that were in excess of the expected age. Natural infrared-stimulated luminescence (IRSL) intensities as well as single grain palaeodoses show a wide range of values. Most of the bright grains yield equivalent doses largely in excess of the expected palaeodose, considering the depositional age of the sample. The luminescence emitted by the brightest grains would dominate the signal emitted from aliquots containing many grains. This explains the overestimation of ages obtained using standard luminescence techniques for the sample investigated. Palaeodoses obtained from grains that exhibit low IRSL intensities are close to the expected dose. However, the age derived from these grains is lower than the expected age. Anomalous fading is believed to be the main cause for the age underestimation. This study is the first demonstration of the feasibility of dating a sedimentary event using the luminescence of a single mineral grain.     

Radiation effect on the 400-nm-thermoluminescence emission of a potassium-rich feldspar

The UV-blue thermoluminescence (TL) emission of exsolved and twinned potassium feldspars is potentially valid to be employed in the field of dating and retrospective dosimetry. This paper reports about the following results: (i) The dose dependence of the 400 nm TL intensity of a K-rich feldspar exhibits an excellent linearity in the range of 50 mGy–8 Gy. (ii) The stability of the TL signal after 6 months of storage, shows an initial rapid decay (ca. 45%) maintaining the stability from 40 days onwards which indicates that the electron population decreases asymptotically by the X-axis and the involved electrons are located in deeper traps at room temperature. The fading process can be fitted to a first-order decay equation of the sort y=y₀+A exp(−x/t). (iii) The tests of thermal stability at different temperatures confirm a continuous trap distribution with progressive changes in the glow curve shape, intensity and temperature position of the maximum peak. According to this behaviour some physical parameters are defined.     

Formation of epitaxial SiC nanocrystals

Epitaxial 3C-SiC grains are formed at 1190 °C in the top region of silicon, when Si wafers coated by SiO₂ are annealed in CO atmosphere. The formed SiC grains are 40-50 nm high and 100 nm wide in cross-section and contain only few defects. Main advantage of the method is that the final structure is free of voids.The above method is further developed for the generation of SiC nanocrystals, embedded in SiO₂ on Si, and aligned parallel with the interface. The nanometer-sized SiC grains were grown into SiO₂ close to the Si/SiO₂ interface by a two-step annealing of oxide covered Si: first in a CO, than in a pure O₂ atmosphere. The first (carbonization) step created epitaxial SiC crystallites grown into the Si surface, while the second (oxidation) step moved the interface beyond them. Conventional and high resolution cross-sectional electron microscopy showed pyramidal Si protrusions at the Si/SiO₂ interface under the grains. The size of the grains, as well as their distance from the Si/SiO₂ interface (peak of pyramids) can be controlled by the annealing process parameters. The process can be repeated and SiC nanocrystals (oriented in the same way) can be produced in a multilevel structure.     

A comparative study of the luminescence characteristics of polymineral fine grains and coarse-grained K- and Na-rich feldspars

The IRSL and post-IR IRSL (pIRIR) signal characteristics of polymineral fine grains are investigated and compared with those of K- and Na-rich feldspar extracts. TL signal loss after IR and pIRIR stimulations occurs mainly at around 320 °C for polymineral and Na-feldspar samples and around 410 °C for K-feldspar samples, when a preheat temperature of 250 °C for 60 s is used. After preheating to a higher temperature (320 °C for 60 s) all samples show a TL reduction around 410 °C in the blue detection window. Pulse annealing experiments for IRSL and pIRIR signals for preheats between 320 °C and 500 °C indicate that the signal stabilities are similar among the different feldspar types, when a higher preheat temperature (>320 °C) is used. Thermal activation energies for IRSL and pIRIR signals are largest in K-feldspar and smallest in polymineral fine grains, in both blue and UV detection windows for both fast time-resolved (TR) and continuous wave (CW) signals. These results suggest that IRSL and pIRIR signals in polymineral fine grains originate mainly from Na-feldspar grains; these signals are less thermally stable than those from K-feldspar, but a more stable signal (presumably from K-feldspar grains) can be obtained using a higher preheat temperature.