SPM Analysis of Firing Technology on Ru · PDF file306.2 Proceedings of the 10th International...
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10th International Conference on Particle Induced X-ray Emission and its Analytical Applications PIXE 2004, Portorož, Slovenia, June 4-8, 2004 http://pixe2004.ijs.si/
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SPM Analysis of Firing Technology on Ru Porcelain Feng Songlin, Feng Xiangqian, Cheng Lin, Lei Yong, Xu Qing
Institute of High Energy Physics, Chinese Academy of Sciences, P. O. Box 918, Beijing 100039, P. R. China
Milko Jakšić
Ruđer Bošković Institute, Zagreb, Croatia
ABSTRACT
The firing technology of various cooling modes was adopted for copying the glaze color of ancient Ru ware, which was one of the most famous ancient porcelain in Song dynasty (960 A.D.∼1276 A.D.) of China. The glaze color depended on the cooling process in this work. The elemental distribution in the glaze surface was analyzed by Scanning Proton Microscope (SPM). The results indicated that: the elemental distribution of copied Ru porcelain is inhomogeneous which was rapidly cooled from 900°C to room temperature, but it is uniform for the nature cooling mode
Keywords: Ru porcelain; firing technology; elemental distribution; glaze color; SPM Corresponding author: Feng Songlin; [email protected]
1. INTRODUCTION
Ru ware [1] is one of the most famous ancient porcelain in Song Dynasty (960 A.D.∼1276 A.D.) of China. It was a kind product made from Ru kiln in Henan Province of China. The Ru kiln is one of the five most famous kiln sites that were controlled by court. Especially, the Ru ware which with glaze color of sky blue was only supplied to the palace and minister. Altogether, the amounts of the ancient Ru wares are not more than three hundred in the whole world today. It is the kind porcelain that most archeologists, collectors and the fancier enjoy.
The ceramic experts and copying makers have being copied it with various methods and technology for longer time. Many materials with different chemical composition and content were used to copy the glaze color of Ru porcelain. Some different firing temperatures and their rising process were adopted. However, the color and seeing effect of copying glaze is not entirely similar with ancient Ru ware. At present, new firing technology of various cooling modes have being adopted and studied further [2, 3]. After reached the firing temperature and remained it for certain time, the body and glaze material became pre-crystallizing glass state. The hot porcelain is cooled in various processes at different temperature. One way is that the hot porcelain with firing temperature was directly taken out of stove and cooled in air. Other process is that the hot porcelain was being cooled to various temperatures in oven, and then took it out and remained in air. The glaze color became from light blue to dark one. The color and its seeing effect of copying glaze were much better.
The elemental distribution in surface of copying Ru porcelain sample with different cooling process was analyzed by Scanning Proton Microscope (SPM), in order to analyze the effects of chemical composition and research its firing technology [4].
2. EXPERIMENTAL
All the glaze materials of copying Ru porcelain samples were made from same chemical composition and concentration in this paper. The samples were fired simultaneously in a stove with same condition. It was remained several hours as the stove temperature risen to about 1250 0C. Some samples were cooled to 900 0C within 1 hr, 800 0C in 2.5 hr, and 200 0C for 24 hr respectively in furnace, and then moved it out and remained in air. However, several specimens were cooled to room temperature in
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Proceedings of the 10th International Conference on Particle Induced X-ray Emission and its Analytical Applications , Portorož, Slovenia, June 4-8, 2004
stove all the time, it is about 48 hr. The glaze color became from light blue to dark one. The color and its seeing effect of copying glaze were familiar with ancient ones. The analyzed samples were shown as in table 1.
TABLE.1 The glaze color and cooling temperature
Samples Glaze color Cooling temperature and process HNRF005 Blue sky Cooling in stove HNRF006 Blue with lighter yellow Cooling in air from 200 0C HNRF007 Blue with light yellow Cooling in air from 800 0C HNRF008 Blue with yellow Cooling in air from 900 0C
The experiment of the elemental distribution in glaze surface was performed in the SPM
laboratory of Ruđer Bošković Institute, Zagreb, Croatia. The diameter of beam spot was 1 µm with a proton energy of 2.4 MeV and beam current of 2 nA. A scanning region of 500×1000 µm2 was used in the experimental system.
3. RESULTS AND DISCUSSION
Si Al K Ca Fe
FIGUER 1. Elemental distribution in sample HNRF005 surface
Si Al K Ca Fe FIGURE 2. Elemental distribution in sample HNRF006 surface
Si Al K Ca Fe FIGURE 3. Elemental distribution in sample HNRF007 surface
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Proceedings of the 10th International Conference on Particle Induced X-ray Emission and its Analytical Applications , Portorož, Slovenia, June 4-8, 2004
Si Al K Ca Fe FIGURE 4. Elemental distribution in sample HNRF008 surface
These distribution plots of major elements of Si, Al, K, Ca and Fe are shown in this paper,
because the concentrations of Ti, Mn, Cu, Zn and etc are lower in the glaze and no obvious variations have been observed. The distribution of main elements of sample HNRF005 cooled in the stove is shown in Fig.1. The elemental distribution in glaze surface was nearly homogeneous. A little distribution variation of Al and Ca occurred in sample HNRF006 as shown in Fig.2, which was cooled to 200 0C in furnace and remained in air. The variations in distribution of Al and Ca were obviously in sample HNRF007 as shown in Fig.3, which was cooled to 700 0C in stove and then remained in air. The variations of Al and Ca were clearer in sample HNRF008 as shown in Fig.4, which was cooled to 900 0C and then moved directly in air.
4. CONCLUSION
Generally, The crystallizing process was going with the falling course of stove temperature. The more sufficient the crystallization of the glaze, the lower the cooling temperature of the furnace. Therefore, the elemental distribution was inhomogeneous. In other words, the higher the cooling temperature which the hot porcelain moved out from the stove, the much homogeneous the elements distributed. However, The results indicated that the elemental distribution of glaze surface of copied Ru porcelain is inhomogeneous which was rapidly cooled from 900°C to room temperature, but it is uniform for the nature cooling mode. The glaze color is depended on the microstructure, chemical composition and firing technology, which is key factor worth to study further.
ACKNOWLEDGMENTS
The authors appreciate the financial support by the Intellectual Creative Engineering of Chinese Academy of Sciences ( KJCX-N04), the National Natural Science Foundation of China (10135050&10275016).
REFERENCES
1. Li, J. Z.: A History of Science and Technology in China (Vol.Ceramics ) Beijing: Science Press(1998) (in Chinese)
2. Huang, Y. Y., Zhao, L. M. and Wang, Z. G.: International Journal of PIXE. 9. 175-180(1999) 3. Huanshen Cheng and Wenquan He, NIM-B118, P377-380(1996) 4. Feng Songlin, Zhong Min, Ren Minqin etc, NIM-B75, P375-378(1993)