{"title":"熔体粘度测定的DSC移位因子法的实验室内校准:以偏硅酸铅玻璃为例","authors":"Danilo Di Genova , Gabriele Giuliani , Sumith Abeykoon , Kajal Dadwal , Suruchi Sharma , Atul Khanna , Alessio Zandonà , Dmitry Bondar , Stefanie Meyer , Laura Calabrò , Serena Dominijanni , Joachim Deubener","doi":"10.1016/j.jnoncrysol.2025.123709","DOIUrl":null,"url":null,"abstract":"<div><div>The differential scanning calorimetry (DSC) shift-factor approach provides a powerful tool for determining the shear viscosity of glass-forming melts across several orders of magnitude. Its accuracy, however, depends on the proper determination of the shift factor (<em>K</em>) – a process of establishing <em>K</em> by linking DSC data to viscometry, herein termed 'intralaboratory calibration' – which then connects the fictive temperature to viscosity. In this study, we determine <em>K</em> for lead metasilicate (PbSiO<sub>3</sub>) glass by integrating conventional DSC, flash DSC, and ball penetration viscometry measurements on samples obtained from the same batch. Raman spectroscopy was employed to verify sample integrity before and after measurements.</div><div>Our results confirm the applicability of the DSC shift-factor approach, yielding shift factors of <em>K<sub>onset</sub></em> = 10.92 ± 0.04, <em>K<sub>peak</sub></em> = 9.41 ± 0.08, and <em>K<sub>endset</sub></em> = 8.71 ± 0.07. These findings underscore the importance of intralaboratory calibration in refining the DSC-based method for accurate viscosity determination in glass-forming systems.</div></div>","PeriodicalId":16461,"journal":{"name":"Journal of Non-crystalline Solids","volume":"666 ","pages":"Article 123709"},"PeriodicalIF":3.5000,"publicationDate":"2025-08-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"Intralaboratory calibration of the DSC shift-factor approach for melt viscosity determination: A case study on lead metasilicate glass\",\"authors\":\"Danilo Di Genova , Gabriele Giuliani , Sumith Abeykoon , Kajal Dadwal , Suruchi Sharma , Atul Khanna , Alessio Zandonà , Dmitry Bondar , Stefanie Meyer , Laura Calabrò , Serena Dominijanni , Joachim Deubener\",\"doi\":\"10.1016/j.jnoncrysol.2025.123709\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<div><div>The differential scanning calorimetry (DSC) shift-factor approach provides a powerful tool for determining the shear viscosity of glass-forming melts across several orders of magnitude. Its accuracy, however, depends on the proper determination of the shift factor (<em>K</em>) – a process of establishing <em>K</em> by linking DSC data to viscometry, herein termed 'intralaboratory calibration' – which then connects the fictive temperature to viscosity. In this study, we determine <em>K</em> for lead metasilicate (PbSiO<sub>3</sub>) glass by integrating conventional DSC, flash DSC, and ball penetration viscometry measurements on samples obtained from the same batch. Raman spectroscopy was employed to verify sample integrity before and after measurements.</div><div>Our results confirm the applicability of the DSC shift-factor approach, yielding shift factors of <em>K<sub>onset</sub></em> = 10.92 ± 0.04, <em>K<sub>peak</sub></em> = 9.41 ± 0.08, and <em>K<sub>endset</sub></em> = 8.71 ± 0.07. These findings underscore the importance of intralaboratory calibration in refining the DSC-based method for accurate viscosity determination in glass-forming systems.</div></div>\",\"PeriodicalId\":16461,\"journal\":{\"name\":\"Journal of Non-crystalline Solids\",\"volume\":\"666 \",\"pages\":\"Article 123709\"},\"PeriodicalIF\":3.5000,\"publicationDate\":\"2025-08-11\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Journal of Non-crystalline Solids\",\"FirstCategoryId\":\"88\",\"ListUrlMain\":\"https://www.sciencedirect.com/science/article/pii/S0022309325003254\",\"RegionNum\":3,\"RegionCategory\":\"材料科学\",\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"Q1\",\"JCRName\":\"MATERIALS SCIENCE, CERAMICS\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Journal of Non-crystalline Solids","FirstCategoryId":"88","ListUrlMain":"https://www.sciencedirect.com/science/article/pii/S0022309325003254","RegionNum":3,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q1","JCRName":"MATERIALS SCIENCE, CERAMICS","Score":null,"Total":0}
Intralaboratory calibration of the DSC shift-factor approach for melt viscosity determination: A case study on lead metasilicate glass
The differential scanning calorimetry (DSC) shift-factor approach provides a powerful tool for determining the shear viscosity of glass-forming melts across several orders of magnitude. Its accuracy, however, depends on the proper determination of the shift factor (K) – a process of establishing K by linking DSC data to viscometry, herein termed 'intralaboratory calibration' – which then connects the fictive temperature to viscosity. In this study, we determine K for lead metasilicate (PbSiO3) glass by integrating conventional DSC, flash DSC, and ball penetration viscometry measurements on samples obtained from the same batch. Raman spectroscopy was employed to verify sample integrity before and after measurements.
Our results confirm the applicability of the DSC shift-factor approach, yielding shift factors of Konset = 10.92 ± 0.04, Kpeak = 9.41 ± 0.08, and Kendset = 8.71 ± 0.07. These findings underscore the importance of intralaboratory calibration in refining the DSC-based method for accurate viscosity determination in glass-forming systems.
期刊介绍:
The Journal of Non-Crystalline Solids publishes review articles, research papers, and Letters to the Editor on amorphous and glassy materials, including inorganic, organic, polymeric, hybrid and metallic systems. Papers on partially glassy materials, such as glass-ceramics and glass-matrix composites, and papers involving the liquid state are also included in so far as the properties of the liquid are relevant for the formation of the solid.
In all cases the papers must demonstrate both novelty and importance to the field, by way of significant advances in understanding or application of non-crystalline solids; in the case of Letters, a compelling case must also be made for expedited handling.