热重分析技术及其在高分子表征中的应用  

Thermogravimetric Analysis and Its Applications in Polymer Characterization

作　　者：谢启源 陈丹丹 丁延伟 Qi-yuan Xie;Dan-dan Chen;Yan-wei Ding(State Key Lab of Fire Science;Instruments Center for Physical Science,University of Science and Technology of China,Hefei 230026)

机构地区：[1]中国科学技术大学火灾科学国家重点实验室 [2]中国科学技术大学合肥微尺度物质科学国家研究中心,合肥230026

出　　处：《高分子学报》2022年第2期193-210,共18页Acta Polymerica Sinica

基　　金：国家重点研发计划专项(项目号2020YFC1522800);中央高校基本科研业务费专项资金(项目号WK2320000043,WK2320000047)资助项目.

摘　　要：热重分析技术(TGA)是在程序控制温度和设定气氛下表征材料受热过程中的质量随温度或时间变化的高精度研究工具,具有重复性好、灵敏度高和热过程控制精准等优点.近年来,TGA技术在高分子材料领域得到了广泛应用,促进了高分子材料热稳定性、组成分析以及热分解机理等材料细观热响应特性的深入研究.本文分别从热重分析基本原理、仪器校准、实验方案设计、实验操作、热重曲线综合解析以及各环节中易出现的不当操作、异常数据与解决方案等方面进行阐述,并给出了在高分子科学研究领域中的典型应用案例、未来发展趋势及机遇与挑战.在实际应用中,基于TGA与傅里叶红外光谱(FTIR)、示差扫描量热法(DSC)、气相色谱-质谱联用(GC/MS)等技术的联用分析,将有利于进一步揭示高分子材料在不同气氛和热激励等条件下的详细热响应信息,为性能优异的新型高分子材料研发与设计、热解机理及燃烧蔓延动力学等领域提供支撑和指导.Thermogravimetric analysis(TGA)is an efficient research tool that characterizes the weight of materials with temperature or time under a program controlled temperature and a certain atmosphere.One of its advantages is that the TGA results can be well repeated with high sensitivity.In addition,its heating process is accurately and flexibly controlled according to real thermal environment of samples.In recent years,TGA is popularly used in the field of polymer materials,which promotes the detailed analyses on their thermal stability,composition analysis and thermal decomposition mechanism et al.This review covers many aspects of TGA,including basic principles,calibration,scheme design,curve analysis,as well as those common errors during sample preparation and experiments,abnormal data figuring and the solution to them.Additionally,the typical application cases of TGA in polymer science,as well as their opportunity and challenges in future,are also presented.In the applications of TGA technology,more information about the thermal-response behavior of polymers under different atmosphere and heating conditions could be revealed by TGA coupled with FTIR,DSC,GC/MS technologies.In this case,not only the weight information of sample during a specific heating condition,but also the endothermic and exothermic behaviors,released gas components at the same time can be analyzed together.They are helpful for new polymer design,thermal decomposition mechanism and flame spread models development.

关 键 词：热重分析技术 曲线解析 热稳定性 热解机理 案例分析 

分 类 号：TQ317.2[化学工程—高聚物工业]