示差扫描量热法进展及其在高分子表征中的应用

陈咏萱; 周东山; 胡文兵

doi:10.11777/j.issn1000-3304.2020.20234

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示差扫描量热法进展及其在高分子表征中的应用

综述 (高分子表征技术专题) | 更新时间：2021-03-05

- 示差扫描量热法进展及其在高分子表征中的应用
- Progress of Differential Scanning Calorimetry and Its Application in Polymer Characterization
- 高分子学报 2021年52卷第4期页码：423-444
- 作者机构：
  
  南京大学化学化工学院配位化学国家重点实验室　南京 210023
- 作者简介：
  
  [ "胡文兵，男，1966年生. 南京大学化学化工学院高分子系教授、博士生导师. 1989年本科毕业于复旦大学材料科学系，1995年博士毕业于复旦大学高分子科学系. 分别于1998~1999年赴德国弗莱堡大学物理系、2000~2001年美国田纳西大学化学系、2001~2003年荷兰物质科学研究院(FOM)原子与分子物理研究所从事博士后研究. 2004年至今，在南京大学任教. 2008年获杰出青年科学基金资助，2020年入选美国物理学会会士(APS Fellow). 主要研究方向为采用蒙特卡洛分子模拟和Flash DSC研究高分子结晶机理及材料热导率表征" ]
- 基金信息：
  
  国家自然科学基金(基金号 21973042)资助项目()
- DOI：10.11777/j.issn1000-3304.2020.20234
  中图分类号：
- 纸质出版日期：2021-4-3，
  
  网络出版日期：2021-1-6，
  
  收稿日期：2020-10-26，
  
  修回日期：2020-11-17，
扫描看全文
陈咏萱, 周东山, 胡文兵. 示差扫描量热法进展及其在高分子表征中的应用[J]. 高分子学报, 2021,52(4):423-444.

Yong-xuan Chen, Dong-shan Zhou, Wen-bing Hu. Progress of Differential Scanning Calorimetry and Its Application in Polymer Characterization[J]. Acta Polymerica Sinica, 2021,52(4):423-444.
陈咏萱, 周东山, 胡文兵. 示差扫描量热法进展及其在高分子表征中的应用[J]. 高分子学报, 2021,52(4):423-444. DOI： 10.11777/j.issn1000-3304.2020.20234.

Yong-xuan Chen, Dong-shan Zhou, Wen-bing Hu. Progress of Differential Scanning Calorimetry and Its Application in Polymer Characterization[J]. Acta Polymerica Sinica, 2021,52(4):423-444. DOI： 10.11777/j.issn1000-3304.2020.20234.

摘要

示差扫描量热法(DSC)是表征材料热性能和热反应的一种高效研究工具，具有操作简便、应用广泛、测量值物理意义明确等优点. 近年来DSC技术的发展大大拓展了高分子材料表征的测试范围，促进了对高分子物理转变的热力学和动力学的深入研究. 温度调制示差扫描量热法(TMDSC)是DSC在20世纪90年代的标志性进展，它在传统DSC的线性升温速率的基础之上引入了调制速率，从而可将总热流信号分解为可逆信号和不可逆信号两部分，并能测量准等温过程的可逆热容. 闪速示差扫描量热法(FSC)是DSC技术近年来的创新性发展，它采用体积微小的氮化硅薄膜芯片传感器替代传统DSC的坩埚作为试样容器和控温系统，实现了超快速的升降温扫描速率以及微米尺度上的样品测试，使得对于高分子在扫描过程中的结构重组机制的分析以及对实际的生产加工条件的直接模拟成为可能. 本文从热分析基础出发，依次对传统DSC、TMDSC和FSC进行了介绍，内容覆盖其发展历史、方法原理、操作技巧及其在高分子表征中的应用举例，最后对DSC未来的发展和应用进行了展望. 本文希望通过综述DSC原理、实验技巧和应用进展，帮助读者加深对DSC这一常用表征技术的理解，进一步拓展DSC表征高分子材料的应用.

Abstract

Differential scanning calorimetry (DSC) is a highly efficient tool to characterize the thermal properties and to investigate thermal reactions of materials owing to its advantages of simplicity and universality as well as the well-defined measurement results with a clear physical meaning. In recent years

the tremendous development of DSC technique has greatly extended the measurement range for polymer characterization

facilitating the further research on thermodynamics and kinetics of physical transitions in polymer materials. Temperature-modulated DSC (TMDSC)

a remarkable advance in DSC technique in 1990s

introduces scanning rate perturbation into the traditional linear heating rate so that the overall heat flux could be separated into reversible and non-reversible signals and furthermore

the reversing heat capacity could be measured in the quasi-isothermal process. Fast scanning chip-calorimetry (FSC) is a new progress of DSC technique in recent years

which adopts a miniature chip made of silicon nitride thin films to replace the traditional crucible as the sample holder and temperature controller

thus achieving ultra-fast heating and cooling rates for the measurement with sample mass on micro- and nanogram scale

which makes it possible to analyze the structural reorganization phenomena occurring frequently during temperature scanning and to simulate the actual condition of polymer processing. This review starts with the fundamentals of thermal analysis

followed with a sequential introduction of DSC

TMDSC and FSC by covering their histories

principles

experimental skills as well as their practical examples of polymer characterization. In the end

the prospects of the development and application of DSC are highlighted. We hope this survey would help the readers to gain a deeper understanding of the commonly used DSC technique and encourages them to expand further applications of DSC techniques in polymer characterization.

关键词

高分子表征示差扫描量热法温度调制示差扫描量热法闪速示差扫描量热法

Keywords

Polymer characterizationDifferential scanning calorimetryTemperature-modulated DSCFast scanning chip-calorimetry

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