Morphological and structural study of crystals in black-to-brown glazes of Yaozhou ware (Song dynasty) using imaging and spectroscopic techniques

Holé, Clément; Ren, Zhao; Zhang, Pei; Shi, Pengfei; Zhu, Jianfeng; Luo, Hongjie; Fen, Wang; Sciau, Philippe

doi:10.1016/j.jeurceramsoc.2021.05.025

Cited by 15 publications

(5 citation statements)

References 22 publications

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“…The underlying third one contained a significant level of crystals smaller than those found in first sublayer and showed gradient variation tendency on shape and size as deeper in the glaze. Such similar layered structure has been already reported in the studies of sauce glaze from the Qilizhen kilns and brown glaze from the Yaozhou kilns 14,29 …”

Section: Resultssupporting

confidence: 83%

“…Such similar layered structure has been already reported in the studies of sauce glaze from the Qilizhen kilns and brown glaze from the Yaozhou kilns. 14,29 Figure 6A presented the SEM image of OS glaze surface within the area of a silvery spot. It was covered by the intensive branch-like and leafy crystals with sizes varying from 1 to 20 μm in diameter, indicating a large heterogeneity of iron supersaturation in this area (Figure 6B).…”

Section: Microstructure Analysis By Semmentioning

confidence: 99%

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Morphological and structural analysis of iron‐rich porcelains excavated from the Jian kiln site of Song dynasty

Tao,

Liu,

Dong

et al. 2023

Journal of Microscopy

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Iron‐rich porcelains generally embrace relatively high iron concentration in the glaze and body, which have an important position in the history of ancient Chinese high‐temperature ceramics. The colour and lustre of glaze patterns are closely related to the orientation and order of crystallisation. In this work, three representative types of iron‐rich porcelains (persimmon red‐glazed sample, oil spot‐glazed sample and mirror black‐glazed sample) were analysed by portable energy‐dispersive X‐ray fluorescence (PXRF), optical coherence tomography (OCT), optical microscopy (OM), scanning electron microscopy (SEM), X‐ray diffraction (XRD) and laser Raman spectroscopy (RS) to determine the morphology, chemical composition and microstructure. Results showed that layered structure was observed in both persimmon red and oil spot glazes, however with respective thickness. Besides, iron‐enriched crystals mostly precipitated on glaze surface. For the persimmon red sample, multilayer microstructure consisting of three sublayers beneath glaze surface was identified. Crystals and dark red substrates were all made of ε‐Fe2O3, implying that it was fired at a strong reducing atmosphere. But for the oil spot sample, large‐scale leaf‐shaped crystals were well characteristic of ε‐Fe2O3, while small snowflake‐shaped crystals were assigned to α‐Fe2O3, indicating that the firing environment was partially reduced. In addition, there was no crystalline layer existing on surface of mirror black‐glazed porcelain, and plain black glaze layer was featured by a glassy matrix.The Jian kiln is a famous ancient folk kiln in the southern China that is currently located in Jianyang county of Fujian province. Its production of black‐glazed porcelain began in the Tang dynasty (618–907 AD), became prosperous in the Southern Song dynasty (1127–1279 AD), and declined and ended in the Yuan dynasty (1271–1368 AD). Black‐glazed Jian tea bowls were perfect for highlighting the rich white tea decoction. The thick and lustrous black glaze of Jian bowls sometimes were featured by streaked or mottled patterns, usually recognised by ‘hare's fur (HF)’, ‘oil spot (OS)’, ‘partridge spot (PS)’ and so on, which were the crystalline markings of iron oxide precipitated during firing in the dragon kiln. Iron oxide acted as a colorant for black‐glazed porcelain and, thus, was called as iron‐rich porcelain. The unique patterns originated from local iron‐enrichment raw materials and firing process, and the locally iron‐enriched areas generated due to the supersaturated crystallisation of different iron oxide in the cooling period. It was generally believed that research studies on the crystallographic nature and growth mechanism of surface crystals would provide help for the manufacturing of ancient Chinese glazes. With this aim, three types of iron‐rich porcelain excavated from the Jian kiln were selected to further study the forming cause and growth process of glaze patterns using a series of characterisation methods, like portable energy‐dispersive X‐ray fluorescence (PXRF), optical coherence tomography (OCT), optical microscopy (OM), scanning electron microscopy (SEM), X‐ray diffraction (XRD) and laser Raman spectroscopy (RS).

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Section: Resultssupporting

confidence: 83%

Section: Microstructure Analysis By Semmentioning

confidence: 99%

Morphological and structural analysis of iron‐rich porcelains excavated from the Jian kiln site of Song dynasty

Tao,

Liu,

Dong

et al. 2023

Journal of Microscopy

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“…Although pure "-Fe 2 O 3 particles have sizes reported to be in the nano range, particles found in ancient Chinese glazes regularly exceed 1 mm. It has been hypothesized that these impressive sizes are possible due to Al substitution stabilizing the bigger particles (Wang et al, 2021). The possible range of Al substitution in "-Fe 2 O 3 has also been shown to be very wide (Yamada et al, 2012;Nasu et al, 2017).…”

Section: Hematite and Spinelmentioning

confidence: 99%

“…These glazes were much appreciated during the Song period (Crick, 2013) and are still highly regarded today, with some exceptional bowls considered national treasures in Japan (Song Ceramics, 1999). Several studies have been carried out on ancient samples and highlighted typical dendritic micro-and nanostructures (Dejoie et al, 2014;Wang et al, 2019Wang et al, , 2021Wen et al, 2019;Ren et al, 2022). This set of samples was shown to display comparable dendritic structures, which contain two iron oxide polymorphs among other phases: "-Fe 2 O 3 and hematite (�-Fe 2 O 3 ) (Hole ´et al, 2022).…”

Section: Introductionmentioning

confidence: 98%

Study of the epitaxy between ɛ-Fe₂O₃, hematite and spinel in brown-glazed Chinese ceramics using electron diffraction mapping techniques

Holé,

Brunet,

Joulié

et al. 2024

J Appl Crystallogr

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Black-to-brown Chinese ceramics have sparked the interest of material scientists since the widespread discovery of complex dendritic structures containing mainly the rare ɛ-Fe2O3 polymorph in their glazes. This study proposes to tackle this issue using two electron diffraction mapping techniques, transmission Kikuchi diffraction and automated crystal orientation mapping–precession electron diffraction, which have not been fully exploited despite their relevance for studying these structures at the scales of interest. It first demonstrates the efficiency of applying these techniques to characterize the structures at the nanoscale and discusses some limitations that may be encountered, in particular due to the specificity of heritage samples. It then focuses on the crystalline orientations obtained with these techniques, which highlight epitaxial relationships among the crystalline planes (001) of the ɛ-Fe2O3 phase, (0001) of the hematite and (111) of the spinel. Finally, it discusses the growth of such complex multi-phase structures by proposing two possible mechanisms, one based on the transformation of ɛ-Fe2O3 into hematite and spinel, and the other based on the growth of hematite and spinel on already crystallized ɛ-Fe2O3 dendrites. It also compares the dendritic structures of the two modern samples with those found in an ancient sample of Jian ware.

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“…Spectra recording at brown areas (Figure 3A) present very complex Raman features with bands locating around 158, 179, 239, 300, 363, 422, 458, 571, 696, 775, and 1378 cm À1 , consistent with characteristics of ϵ-Fe 2 O 3 , a rare polymorph of iron oxides. [23] Such metastable crystal has been observed in several types of Chinese ancient ceramics, including of the sauce glazed wares excavated in the Qingliang Temple Ruins, [24] the Qilizhen kilns [25] and Yaozhou kilns, [26,27] and purple-gold glazed wares from the Jingdezhen Imperial kilns. [28] Spectra recording at black areas (Figure 3B) show no any crystalline signal but typical characteristics of glassy matrix with two obvious broad bands at $500 and 1000 cm À1 .…”

Section: Crystals In Glazementioning

confidence: 99%

Micro‐structural study of crystals and glassy matrix of black glazed wares from Jian kilns, China (Song Dynasty, AD 960–1279)

Qian

Wang

et al. 2023

J Raman Spectroscopy

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Black glazed wares (Wujin wares) and hare fur's decorated black glazed wares (HF wares) are ones of typical production of Jian kilns, China during Song Dynasty. In this work, Wujin wares and HF wares excavated in Jian kiln complex (Yulinting kilns, Daluhoumen kilns and Luhuaping kilns) were systematically analyzed by optical microscope, X‐ray fluorescence spectroscopy and micro‐Raman spectroscopy. The results show that the index of glassy polymerization (Ip) of Wujin wares is smaller than black areas of HF wares, indicating the higher firing temperature used for HF wares. Several pseudobrookite, rutile, hematite and quartz crystals were detected in glazes of Wujin wares while a great number of ɛ‐Fe2O3 crystals was observed in brown stripes of HF wares. Besides, wares in different kiln sites present obviously differences in bubble distribution and glassy structure, indicating a lower firing temperature used for Yulinting kilns than those of Daluhoumen kilns and Luhuaping kilns.

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Morphological and structural study of crystals in black-to-brown glazes of Yaozhou ware (Song dynasty) using imaging and spectroscopic techniques

Cited by 15 publications

References 22 publications

Morphological and structural analysis of iron‐rich porcelains excavated from the Jian kiln site of Song dynasty

Morphological and structural analysis of iron‐rich porcelains excavated from the Jian kiln site of Song dynasty

Study of the epitaxy between ɛ-Fe₂O₃, hematite and spinel in brown-glazed Chinese ceramics using electron diffraction mapping techniques

Micro‐structural study of crystals and glassy matrix of black glazed wares from Jian kilns, China (Song Dynasty, AD 960–1279)

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Morphological and structural study of crystals in black-to-brown glazes of Yaozhou ware (Song dynasty) using imaging and spectroscopic techniques

Cited by 15 publications

References 22 publications

Morphological and structural analysis of iron‐rich porcelains excavated from the Jian kiln site of Song dynasty

Morphological and structural analysis of iron‐rich porcelains excavated from the Jian kiln site of Song dynasty

Study of the epitaxy between ɛ-Fe2O3, hematite and spinel in brown-glazed Chinese ceramics using electron diffraction mapping techniques

Micro‐structural study of crystals and glassy matrix of black glazed wares from Jian kilns, China (Song Dynasty, AD 960–1279)

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Study of the epitaxy between ɛ-Fe₂O₃, hematite and spinel in brown-glazed Chinese ceramics using electron diffraction mapping techniques