硅酸盐学报

浑源窑黑釉剔花与黑釉瓷物化组成与制备工艺

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王甜 ¹ , 宋思樾 ¹ , 王秀玲 ² , 侯亮亮 ³ , 王芬 ¹ , 王莹 ¹ , 李强 ⁴^,⁵ , 罗宏杰 ⁵^,¹ , 朱建锋 ¹

硅酸盐学报 | 研究论文 2025,53(1): 125-135

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硅酸盐学报 |研究论文 2025 , 53 (1) : 125 -135

浑源窑黑釉剔花与黑釉瓷物化组成与制备工艺

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王甜¹, 宋思樾¹, 王秀玲², 侯亮亮³, 王芬¹, 王莹¹, 李强⁴^,⁵, 罗宏杰⁵^,¹, 朱建锋¹

作者信息

^1．陕西科技大学材料科学与工程学院，文物保护科学与技术学院，西安 710021

^2．山西大同大学云冈学学院，山西大同 037000

^3．山西大学考古文博学院，太原 030006

^4．中国科学院上海硅酸盐研究所，上海 200050

^5．硅酸盐质文物保护教育部重点实验室（上海大学），上海 200444

通讯作者:

王甜（1988—），女，博士，副教授；

朱建锋（1973—），男，博士，教授。

作者简介:

王甜（1988—），女，博士，副教授。

Composition and Micro-Structure of Black-Glazed Carving Wares and Black Glazed Waves of Hunyuan Kiln

Tian WANG¹, Siyue SONG¹, Xiuling WANG², Liangliang HOU³, Fen WANG¹, Ying WANG¹, Qiang LI⁴^,⁵, Hongjie LUO⁵^,¹, Jianfeng ZHU¹

Affiliations

^1.School of Conservation Science & Technology for Cultural Heritage, School of Material Science & Engineering, Shaanxi University of Science & Technology, Xiʹan 710021, China

^2.School of Yungang, Shanxi Datong University, Datong 037000, Shanxi, China

^3.School of History and Culture, Shanxi University, Taiyuan 030006, China

^4.Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai 200050, China

^5.Key Laboratory of Silicate Cultural Relics Conservation (Shanghai University), Ministry of Education, Shanghai 20444, China

Corresponding Author:

WANG Tian (1988-), female, Ph.D., Associate Professor;

ZHU Jianfeng (1973-), male, Ph.D., Professor. E-mail: zhujf@sust.edu.cn

WANG Tian (1988-), female, Ph.D., Associate Professor. E-mail: wangtian@sust.edu.cn

出版时间: 2025-01-20 doi: 10.14062/j.issn.0454-5648.20240526

文章导航

摘要

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通过对比研究浑源窑黑釉剔花瓷与黑釉瓷的胎釉微观形貌、晶体种类及分布、釉玻璃相结构及釉中铁元素价态，解析胎釉的原料特点与釉的呈色机理，揭示剔花瓷与黑釉瓷的制备工艺的异同。结果表明：二者胎釉采用相似原料与烧成工艺，但剔花瓷釉中更高的CaO，在胎釉结构处分布的钙长石结晶层，有效增加了花纹与胎体的结合性；黑釉剔花瓷胎相对釉具有更高浓度TiO₂和更低浓度MnO₂与Fe₂O₃，使得剔花装饰形成强烈的黑白对比，具有浮雕之感。釉面分布的枝状ε-Fe₂O₃晶体，有效提高了釉面光泽度，进一步增强了装饰效果。此外，釉面还发现少量黑色镁铁尖晶石。

关键词

浑源窑 / 黑釉剔花瓷 / 原料特征 / 制备工艺 / 显微共聚焦Raman光谱

Abstract

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Introduction

Datong, located in the northern of Shanxi province of China, has an important transportation hub, connecting the Central Plains and Inner Mongolia. Various cultures converge in Datong and form rich aesthetics, reflecting in the famous carving black-glazed wares produced during Jin and Yuan Dynasties in Hunyun kilns located in Hunyuan county, Datong. The carving wares are characterized by gray-white body decorated with carved black glazed patterns. Such a gray-white and black contrast gives the patterns a relief-like decoration. Many researches were devoted to analyze regional features, decorative themes and technology of black-glazed carved wares by conventional archaeological methods. Wang et al. investigated one piece of black-glazed carved ware by micro-Raman spectroscopy and found a large number of ε-Fe₂O₃, a few hematite and magnesio-ferrite on the glaze surface, leading to the brown tune of the carved black patterns. However, the lack of the microstructure, chemical and mineral composition of carved black-glazed wares leads to the raw materials and firing protocol of black glazed carving wares, and its relationship to ordinary pure black glazed is still unclear. In this work, carved black-glazed wares and pure black glazed wares of Hunyuan kilns were investigated by a series of analytical techniques. The characteristic of raw materials and firing protocol of black glazed carving ware and its relationship to black glazed ware were discussed.

Methods

Eleven fragments were excavated from Jiezhuang village, Hunyuan county, Datong, China, which could be dated to Jin and Yuan Dynasties according to the archaeological layer. The fragments were prepared as cross-sections by a cold mounting method. The details were described in elsewhere. The morphology, chemical composition, mineral composition and valence state of colorant elements of glaze and body were measured by a model VXH-7000 optical microscope (OM, KEYENCE Co., Japan), a model XGT-7200 X-ray fluorescence (XRF, Horiba Co., Japan), a model Renishaw-invia micro-Raman spectroscope (micro-RS, UK), a model TD3500 Macro-X-ray diffracometer (macro-XRD, Dadong Co, China) and a model Axis Supra X-ray photoelectron spectroscope (XPS, Shimadzu Co., Japan).

Results and discussion

The results by XRF analysis show that the raw materials used for glazes and bodies of carved black-glazed wares and pure black-glazed wares are similar except for the glaze of former, which is much richer in CaO. A higher CaO can enhance the adhesion of the glaze and body. Besides, the bodies are composed of higher TiO₂ and lower MnO₂ and Fe₂O₃ rather than the glazes, leading a gray-white and dark black contrast between the bodies and glazes. The glaze surfaces contain massive dendrite ε-Fe₂O₃ crystals and a few of hematite, magnetite and magnesioferrite. A few of zircon, anorthite, pseudobrookite and quartz appear in the glaze cross-sections. The bodies contain cristobalite, quartz and mullite. There is no obvious difference in the raw materials of carved black-glazed wares and pure black-glazed wares. The degrees of the glassy polymerization (I_p) of carved black glaze and pure black glaze are similar, i.e., 1.34-2.25, which are consistent with the glaze modifiers/network formers mole ratios, i.e., 0.12-0.2. The similar I_p values and mole ratios indicate that the wares both are prepared at the similar firing temperature. Most of carved-black glazed wares and black glazed wares present the similar ratios of iron bivalence and trivalence, i.e., 2.0-2.6, indicating that the wares both are prepared in a reductive atmosphere. Besides, the Raman spectra of the dendrite ε-Fe₂O₃ crystals show an obvious shift to s higher wavenumber possibly due to the lighter ions substituting irons in the crystals to improve their stability. Moreover, the spectra also present different intensity of Raman features, accounting for the different crystal orientation of these crystals. Such a different orientation can make the dendrite crystals react with incident lights in diffractive or reflective function, giving rise to the glaze surface presenting iridescent or silvery effect.

Conclusions

The similar raw materials were used for preparing the carving black-glazed wares and pure black glazed wares expect for the slightly higher CaO in the glazes of carved black glazes. The bodies were composed of higher TiO₂ and lower MnO₂ and Fe₂O₃ rather than the glazes, leading to a gray-white and dark black contrast between the bodies and glazes. The wares both were fired at the similar firing temperature and in a reductive atmosphere. The main minerals of the bodies were cristobalite, quartz and mullite. Numerous dendrite crystals in micron-size with different crystal orientation were distributed in the glaze surfaces, which could react with incident light in diffractive and reflective functions, leading to the glaze presenting iridescence or silver. Besides, a few of magnetite, magnesioferrite, zircon, anorthite, pseudobrookite and quartz were detected in the glazes.

Key words

Hunyuan Kiln / black glazed waves / feature of raw materials / preparation process / micro-Raman spectroscopy

引用本文

王甜, 宋思樾, 王秀玲, 侯亮亮, 王芬, 王莹, 李强, 罗宏杰, 朱建锋. 浑源窑黑釉剔花与黑釉瓷物化组成与制备工艺. 硅酸盐学报, 2025 , 53 (1) : 125 -135 . DOI: 10.14062/j.issn.0454-5648.20240526

Tian WANG, Siyue SONG, Xiuling WANG, Liangliang HOU, Fen WANG, Ying WANG, Qiang LI, Hongjie LUO, Jianfeng ZHU. Composition and Micro-Structure of Black-Glazed Carving Wares and Black Glazed Waves of Hunyuan Kiln[J]. Journal of the Chinese Ceramic Society, 2025 , 53 (1) : 125 -135 . DOI: 10.14062/j.issn.0454-5648.20240526

基金

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国家自然科学基金(62205191; 52272019; 52272020)
陕西省自然科学基础研究计划(2023WGZJ-YB-45; 2024WZ-YBXM-07)
陕西省教育厅重点科学研究计划项目(2022JY008)
硅酸盐质文物保护教育部重点试验室（上海大学）开放课题(SCRC2024KF02ZD; SCRC2024KF04TS)

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2025年第53卷第1期

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文章信息

doi: 10.14062/j.issn.0454-5648.20240526

接收时间：2024-08-14
首发时间：2026-10-22
出版时间：2025-01-20

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出版历史

收稿日期：2024-08-14
修回日期：2024-09-14

基金

国家自然科学基金(62205191; 52272019; 52272020)

陕西省自然科学基础研究计划(2023WGZJ-YB-45; 2024WZ-YBXM-07)

陕西省教育厅重点科学研究计划项目(2022JY008)

硅酸盐质文物保护教育部重点试验室（上海大学）开放课题(SCRC2024KF02ZD; SCRC2024KF04TS)

作者信息

^1．陕西科技大学材料科学与工程学院，文物保护科学与技术学院，西安 710021

^2．山西大同大学云冈学学院，山西大同 037000

^3．山西大学考古文博学院，太原 030006

^4．中国科学院上海硅酸盐研究所，上海 200050

^5．硅酸盐质文物保护教育部重点实验室（上海大学），上海 200444

通讯作者:

王甜（1988—），女，博士，副教授；

朱建锋（1973—），男，博士，教授。

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https://castjournals.cast.org.cn/joweb/gsyxb/CN/10.14062/j.issn.0454-5648.20240526

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2种不同金属材料的力学参数

科 Family	属数 Number of genus	种数 Number of species	占总种数比例 Percentage of total species (%)	属 Genus	种数 Number of species	占总种数比例 Percentage of total species (%)
鹅膏菌科Amanitaceae	2	11	5.26	鹅膏菌属 Amanita	10	4.78
小菇科 Mycenaceae	2	12	5.74	丝盖伞属 Inocybe	5	2.39
多孔菌科 Polyporaceae	8	14	6.70	蜡蘑属 Laccaria	5	2.39
红菇科 Russulaceae	3	23	11.00	小皮伞属 Marasmius	6	2.87
				小菇属 Mycena	11	5.26
				光柄菇属 Pluteus	5	2.39
				红菇属 Russula	17	8.13
				栓菌属 Trametes	5	2.39

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