顶杆热膨胀法测定低温陶的烧成温度  

Determination of Firing Temperature of Low-Temperature Ceramics by Rod Expansion Method

作　　者：杨长安[1] 曹志超 罗宏杰[1,2] 朱建锋[1] 王芬[1] 张彪[1] 施佩[1] YANG Changan;CAO Zhichao;LUO Hongjie;ZHU Jianfeng;WANG Fen;ZHANG Biao;SHI Pei(School of Materials Science and Engineering,Shaanxi University of Science and Technology,College of Cultural Relics Protection Science and Technology,Key Laboratory of Materials and Technology for Underground Cultural Relics Protection,Ministry of Education,Xi’an 710021,China;School of Cultural Heritage and Information Management,Shanghai University,Key Laboratory of Silicate Cultural Relics Protection,Ministry of Education,Shanghai 200444,China)

机构地区：[1]陕西科技大学材料科学与工程学院,陕西科技大学文物保护科学与技术学院,地下文物保护材料与技术教育部重点实验室,西安710021 [2]上海大学文化遗产与信息管理学院,硅酸盐质文物保护教育部重点实验室,上海200444

出　　处：《硅酸盐学报》2025年第3期640-646,共7页Journal of The Chinese Ceramic Society

基　　金：国家自然科学基金(52102108,52102026);陕西省外国专家服务计划项目(2024WZ-YBXM-17)。

摘　　要：顶杆热膨胀法广泛应用于古陶瓷原始烧成温度的测定,但对于烧成温度低于玻璃相形成温度的低温陶仍需改善。本工作以黏土为原料制备不同烧成温度下的黏土样品,并采用X射线衍射仪、同步综合热分析仪和扫描电子显微镜等进行分析,验证高岭石作为烧成温度标志物的合理性。然后,对不同烧成温度下黏土样品的顶杆热膨胀曲线对应的一阶导曲线上高岭石的脱羟基膨胀峰进行拟合,得到高岭石脱羟基膨胀峰与原始烧成温度的关系曲线。最后,通过已知原始烧成温度的黏土样品验证关系曲线的准确性。本工作为顶杆热膨胀法测定低温陶的烧成温度提供理论和实验基础,并为黏土为原料烧制的低温陶烧成温度的测定提供参考。Introduction Thermal expansion analysis is a most widely used method for determining the firing temperature of ancient ceramics,which infers the original firing temperature of ancient ceramics via analyzing the inflection point of the thermal expansion curve.However,for the pottery at an original firing temperature that is lower than the formation temperature of glass phase,the inflection point on the thermal expansion curve is actually the formation temperature of glass phase rather than original firing temperature.To solve a problem of inaccurate determination of low-temperature pottery firing temperature by a thermal expansion method,clay samples fired at different temperatures were prepared with clay as a raw material,and analyzed by X-ray diffraction(XRD),synchronous comprehensive thermal analyzer(TG-DTA),and scanning electron microscopy(SEM).In addition,the first derivative curve corresponding to the top rod thermal expansion curve of clay samples fired at different temperatures fitted to the dehydroxylation expansion peak of kaolinite,and the relationship curve between the dehydroxylation expansion peak of kaolinite and the original firing temperature was also obtained.Methods A clay as a raw material was processed by grinding,screening,drying,pressing,and sintering at different temperatures.Afterwards,the cylindrical samples with a diameter of 5 mm and a length of 25 mm were prepared with clay by polishing.The thermal behavior of clay raw materials was determined by thermogravimetry-differential thermal analysis(TG-DTA).The chemical composition,phase composition,and microstructure of the raw materials and the samples fired at different temperatures were characterized by X-ray fluorescence spectroscopy(XRF),X-ray diffraction(XRD),and scanning electron microscopy(SEM).The linear expansion or contraction process of the samples during the refiring process at different firing temperatures was tested by a thermal expansion instrument.Results and discussion The XRF spectra show that the chemical composition of r

关 键 词：顶杆热膨胀法 低温陶 烧成温度 高岭石 一阶导 

分 类 号：TB321[一般工业技术—材料科学与工程]