Research paperLuminescence determination of firing temperature of archaeological pure sand related to ancient Dian bronze casting, China
Highlights
► Thermal history of a rare archaeological pure sand sample is studied to investigate ancient Dian bronze casting technique. ► Equivalent annealing temperature of the core sand is determined to range from 550°C to 700°C, based on changes in the TL and OSL characteristics after artificial annealing. ► TL/OSL form a potential method to detect thermal history of fired material.
Introduction
Thermoluminescence (TL) testing of ceramic cores of bronzes from museum collections can be applied to detect ancient artifacts and modern forgeries, as reported by Doreen Stoneham (1995). But when dealing with excavated bronzes, researchers may be interested in topics other than authenticity. One example is the firing temperature of ceramic cores or moulds during original casting processes, which relate to ancient casting techniques.
According to the literature the phenomenon of luminescence sensitivity variations has often been observed in quartz from unheated sand and heated sand. For example, Aitken and Smith, Botter-Jensen and Duller reported that there are large differences in OSL (optically stimulated luminescence) sensitivity between unheated quartz and quartz from heated archaeological samples (Aitken and Smith, 1988; Botter-Jensen and Duller, 1992). Yang and McKeever (1990) reported that an increase in sensitivity can be related to the absorbed radiation dose, and sensitization by heat treatment alone also can be observed. They explained the enhanced OSL sensitivity and phototransferred TL sensitivity as a function of annealing temperature. Lima et al. (2002) reported an investigation on the influence of different thermal treatments on the glow curves of natural quartz samples, and showed that sensitization can be achieved. The main effect is related to the thermal treatment by itself, and annealing increases the sensitivity of the natural quartz samples, especially around the 110° C TL peak. Lai et al. (2008) reported a determination of the effects of thermal treatment on the growth curve shape for OSL of quartz. They claimed that a significant difference in the growth curve shape before and after heating to >370 °C at a heating rate of 1 °C/s (TL was measured) might be used as an indicator to detect the thermal history. In addition, many authors reported an enhanced 210° C TL sensitivity of quartz from pre-exposing the sample to gamma radiation followed by annealing at a high temperature, above 400 °C (David et al., 1976; Bailiff and Haskell, 1983; Haskell et al., 1985; Kaipa and Haskell, 1985; Benny and Bhatt, 1997). Some authors reported that the thermal history of the archaeological artefact and/or an appropriate annealing treatment can be approached by the comparison of the shape of the regenerated TL glow curves obtained after annealing a series of aliquots at different temperatures, with the shape of the natural glow curve or by the use of the dose-plateau test (Spencer and Sanderson, 1994; Roque et al., 2004).
In the present paper, we perform TL and OSL measurements on an archaeological ‘core sand’ and a standard sample after heat treatments at different temperatures in order to investigate the thermal history of the ‘core sand’ by comparing quartz with different thermal historical backgrounds.
Section snippets
Site and samples
The Lijiashan cemetery site is located near the Fuxian Lake (Fuxianhu), and is about 15 km from Jiangchuan city, 40 km south of another principal cemetery site of the ancient Dian kingdom, the famous Shizhaishan site, and 80 km south of Kunming city, the capital of Yunnan province. Excavations at Lijiashan uncovered 27 burials in 1972 and 60 burials in 1991–92 (Figs. 1and 2). These date to the last few centuries BC to the first century AD (Yunnan Provincial Museum, 1975; Yunnan Provincial
Experimental
TL and OSL sample preparation was done under subdued red light in the USTC Archaeometry Laboratory. All samples of AQ and SQ were treated by means of the conventional sample preparation techniques (sieving, HCl, H2O2, HF etching and re-sieving) to obtain 90–150 μm quartz samples. The purity of the quartz extracts was confirmed by IR-test: quartz rarely shows OSL when stimulating with IR (IRSL/BLSL ratios<1%). Then the AQ and SQ samples were divided into subsamples that were thermally treated in
OSL and the 110° C TL sensitivity for the pristine (as received) AQ and SQ samples
The intensities of 110° C TL and OSL for the samples of AQ and SQ samples, without heat treatment, are shown in Fig. 3. As can be seen, the natural SQ samples present no significant change for the 110° C TL and OSL sensitivities, and both the sensitivities are lower than 4. The ‘natural’ AQ samples form a striking contrast. The 110° C TL sensitivity of AQ is about 160 times of SQ samples'. The OSL sensitivity of AQ is about 20 times of SQ samples'. Comparison results of the natural samples
Discussions
The natural ‘core sand’ samples presented a higher sensitivity for 110° C TL and OSL compared with laboratory sand samples in the same test conditions. A possibility suggested by researchers that the increase of the sensitivity from thermal treatment may be related to the creation of [H3O4]0 centers that act as luminescence centers (Lima et al., 2002). Increase in sensitivity could also be related to permutations of Al-(O)H to Al-(O)M centers by post-irradiation thermally activated migrations
Conclusions
Clay core for the so-called piece-mould casting is basically made of natural clay material in ancient Bronze Age China. In our investigation, we found that the pure sand lies in the center of the clay core, like the egg yolk, which has never been found in Chinese archaeology. According to the TL and OSL testing results, we determined that the sand inside the clay core of the Lijiashan bronze cow-shaped ornament has been heated during the casting process in the past, and that the equivalent
Acknowledgements
This work was supported by the National Natural Science Foundation of China (NSFC, No. 41073004). We are grateful to Dr. Shenghua Li for his help in planning the experiments as well as for many stimulating discussions. We are thankful to Professor Xu Liu for his great help during the sampling process. We thank the anonymous reviewer for her/his valuable comments and constructive suggestions.
Editorial handling by: R. Grun
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