Raman study of rusty oil spotted glaze produced in Linfen kilns (Shanxi province, AD 1115–1368)

Wang, Minli; Wang, Fen; Holé, Clément; Cao, Jun; Zhu, Jianfeng; Zhang, Pei; Shi, Pengfei; Sciau, Philippe

doi:10.1002/jrs.6229

Cited by 13 publications

(7 citation statements)

References 22 publications

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“…The majority of the detected Raman peak positions at the spectrum A, B, and C matched well with each other, while few of them shifted slightly due to the faceted aspect of crystal lattice originated from the laser source (λ = 532 nm) and/or phonon confinement effect in our samples [36]. We noticed that spectra of the ε-Fe 2 O 3 phase collected from ancient Fe-rich porcelains were almost the same [10,18,21]. The similarities among Raman spectra taken at "A", "B", and "C" strongly suggested that those three types of crystals clusters shared the same mineral composition.…”

Section: Phase Analysis By Xrd and Rssupporting

confidence: 70%

“…ε-Fe 2 O 3 has become a research hotspot as the chromogenic crystals. Researchers also reported the existence of ε-Fe 2 O 3 polymorph in the oil spot Jian wares [19], sauce glaze porcelain from the Qilizhen kiln [20], rusty-oil-spotted glaze at the Linfen kiln [21] and/or Xiao kiln [22], hare's fur glaze of Jizhou kiln [23], brown glaze porcelain of Yaozhou kiln [24], sauce glaze and black glaze porcelains from Qingliangsi site [25], and purple-gold glaze porcelain from the Forbidden City [26]. It is believed that research studies on the growth mechanism of ε-Fe 2 O 3 in ancient porcelains will provide guidance for the artificial synthesis of this promising material, in addition to having a profound impact on Asian ceramic history.…”

Section: Introductionmentioning

confidence: 99%

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A Microstructural and Compositional Study of ε-Fe2O3 Crystals in the Hare’s Fur Jian Ware

et al. 2022

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The Jian kilns in the present-day Jianyang County of Fujian Province are well known for their thick and lustrous black-glazed porcelain production. The hare’s fur (HF) glazed Jian wares characterized by radial fur-like strips, as one of the most typical representatives of black-glazed tea bowls, originate from phase separation of glaze melt and crystallization of iron oxides. In this study, various techniques were performed on the yellowish-brown HF samples, including portable energy-dispersive X-ray fluorescence (PXRF), synchrotron X-ray absorption near-edge spectroscopy (XANES), optical microscopy (OM), scanning electron microscopy (SEM), X-ray diffraction (XRD) and Raman spectroscopy (RS). The objective of this study was to well understand the microstructure characteristics and chemical compositions of glaze patterns. Results showed that the main constituents of the ceramic glaze were alumina (10.61–16.43 wt.%), silica (62.20–77.07 wt.%), calcium (3.85–6.97 wt.%), and iron oxide (4.10–8.35 wt.%). The studies provided evidence that metastable epsilon-iron oxide crystals (ε-Fe2O3) formed on the brownish-yellow glazed surface. Microstructural analysis revealed that there were three types of crystal structures in the glaze surface: One consisted of well-grown leaf-like or dendritic-like structure with highly ordered branches at micrometers scales; another comprised flower-like clusters accompanied by branches radiating from the center, petals growing along the branches, and needles on both sides of the petals; the last type involved a honeycomb structure tightly packed with plentiful spherical or irregular-shaped particles. In addition, ε-Fe2O3 crystals in the cross-section of the glaze showed a gradient distribution.

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Section: Phase Analysis By Xrd and Rssupporting

confidence: 70%

Section: Introductionmentioning

confidence: 99%

A Microstructural and Compositional Study of ε-Fe2O3 Crystals in the Hare’s Fur Jian Ware

et al. 2022

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“…In previous study of the brown glazed stoneware from Yaozhou kiln, iron oxide crystals with a size of 2–3 μm were found on the glaze surface, as well as large dendritic‐like flakes, which are larger than 25 μm (Wen et al, 2019). Most of the ε‐Fe 2 O 3 crystals found in ancient Chinese stonewares, such as Oil Spot and Hare's Fur Jian ware (Dejoie et al, 2014; Liu et al, 2018), purple‐gold glazed stoneware from the Forbidden City (Wang et al, 2019), sauce glazed and black glazed stonewares from Qingliangsi Site Qilizhen kiln, and Linfen kiln (Wang et al, 2021), are organized in a leaf‐like or dendritic‐like manner. It was also found in the bluish white porcelain from Jingdezhen recently (Hoo et al, 2021).…”

Section: Resultsmentioning

confidence: 99%

Formation mechanism of the pinholes in brown glazed stoneware from Yaozhou kiln

et al. 2021

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Pinhole is a common defect widely seen in many archeological stonewares from different kilns and periods. It is usually a sub‐millimeter pit on the glaze that was believed to be caused by the broken bubbles during the firing process. We investigated the pinholes on a porcelain sherd from Yaozhou kiln of the Song Dynasty (AD 960–1,127), surprisingly, every pinhole corresponds to a flower‐like cluster observed through the microscope. The flower‐like clusters are composed of radial mullite whiskers and ε‐Fe2O3 dendrites, and its growth mechanism were proposed after detailed microscopic and spectroscopic characterizations. The unique chemical composition around the pinholes became the breeding ground for the crystallization of flowers, whereas the crystallization process further facilitates the formation of the pinhole preventing the glaze from restoring smoothness. Our results enriched the knowledge on pinholes and revealed the interesting crystallization assisted formation mechanism, which not only related to bubble rupture but involves the crystallization dynamics as well.

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“…Iron‐rich glaze generally embraced relatively higher iron concentration, and the patterns occurred owing to phase separation between the melted glaze and crystallised iron oxide, which had an important position in ancient Chinese porcelain. Upon firing (1240°C), iron minerals in the melting glaze thermally decompose into iron oxide and oxygen, and iron oxide progressively accumulate around the growing oxygen bubbles, then iron‐enriched areas will form on the glaze surface after larger bubbles ultimately release 35–37 . Phase separation takes place with temperature increases, and the surface iron‐rich (flux) spots begin to flow down along the sides of tea bowls.…”

Section: Discussionmentioning

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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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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Raman study of rusty oil spotted glaze produced in Linfen kilns (Shanxi province, AD 1115–1368)

Cited by 13 publications

References 22 publications

A Microstructural and Compositional Study of ε-Fe2O3 Crystals in the Hare’s Fur Jian Ware

A Microstructural and Compositional Study of ε-Fe2O3 Crystals in the Hare’s Fur Jian Ware

Formation mechanism of the pinholes in brown glazed stoneware from Yaozhou kiln

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

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