热分析资料：DMA在高分子表征中的应用——文献总结

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1、112表征聚合物材料的阻尼性能研究聚合物的固化与交联研究聚合物材料的老化性目录 Contents32所用材料：碳纤维环氧树脂预浸料1.研究聚合物的固化与交联Stark W.Investigation of the curing behaviour of carbon fibre epoxy prepreg by Dynamic Mechanical Analysis DMAJ.Polymer Testing,2013,32(2):231239.Investigation of the curing behaviour of carbon fibre epoxy prepreg by Dynam

2、ic Mechanical Analysis DMA文献一研究思路DMA单悬臂测量设备 碳纤维预浸料样片温度区间：-90280升温速率：1 和 2 K/min正弦刺激31.研究聚合物的固化与交联Fig.1.Prepreg clamped in single cantilever DMA device,fixed wedge on left,oscillating wedge on right.Stark W.Investigation of the curing behaviour of carbon fibre epoxy prepreg by Dynamic Mechanical Anal

3、ysis DMAJ.Polymer Testing,2013,32(2):231239.41.研究聚合物的固化与交联l 样本长度b 试样宽度h 样品厚度F*复杂的受力A*复杂的挠度相位角相位角E 储能模量E 损耗模量 应力幅值 应变振幅Stark W.Investigation of the curing behaviour of carbon fibre epoxy prepreg by Dynamic Mechanical Analysis DMAJ.Polymer Testing,2013,32(2):231239.复数模量5Fig.2.Basic course of storage m

4、odulus E ,loss modulus E and tan as function of t 1.研究聚合物的固化与交联Stark W.Investigation of the curing behaviour of carbon fibre epoxy prepreg by Dynamic Mechanical Analysis DMAJ.Polymer Testing,2013,32(2):231239.tan峰值温度高于损耗模量的峰值温度6Fig.3.Storage modulus E,loss modulus E,tanas function of temperature,mea

5、suring frequency 1 Hz,at a heating rate of 2K/min.1.研究聚合物的固化与交联Stark W.Investigation of the curing behaviour of carbon fibre epoxy prepreg by Dynamic Mechanical Analysis DMAJ.Polymer Testing,2013,32(2):231239.1220总的DMA图谱71.研究聚合物的固化与交联DSC图Fig.4.DSC heat flow and reaction integral as function of tempe

6、rature,at a heating rate of 2 K/min.8Fig.3.Storage modulus E,loss modulus E,tanas function of temperature,measuring frequency 1 Hz,at a heating rate of 2K/min.1.研究聚合物的固化与交联Stark W.Investigation of the curing behaviour of carbon fibre epoxy prepreg by Dynamic Mechanical Analysis DMAJ.Polymer Testing,

7、2013,32(2):231239.1220总的DMA图谱91.研究聚合物的固化与交联Stark W.Investigation of the curing behaviour of carbon fibre epoxy prepreg by Dynamic Mechanical Analysis DMAJ.Polymer Testing,2013,32(2):231239.通过对DSC图谱的分析：在高温区应该有两个峰出现了叠加：Tgmax 和凝胶化转变两步过程Fig.5.tan peak shows no influence by frequency in this temperature

8、region similar as in above.101.研究聚合物的固化与交联Stark W.Investigation of the curing behaviour of carbon fibre epoxy prepreg by Dynamic Mechanical Analysis DMAJ.Polymer Testing,2013,32(2):231239.Fig.5.tan peak shows no influence by frequency in this temperature region similar as in above.通过对DSC图谱的分析：在高温区应该

9、有两个峰出现了叠加：Tgmax 和凝胶化转变111.研究聚合物的固化与交联Stark W.Investigation of the curing behaviour of carbon fibre epoxy prepreg by Dynamic Mechanical Analysis DMAJ.Polymer Testing,2013,32(2):231239.Fig.6.Summary of DMA results,at a heating rate of 2 K/min.121.研究聚合物的固化与交联为了更好地分离理论上的两个峰，尝试了以下研究。.Fig.7.Summary of DMA

10、 results,at a heating rate of 1 K/min.The tan peak is shifted to lower temperature in comparison to the E peak.131.研究聚合物的固化与交联冷却DMA谱图降温曲线对比.Tan向高温移动Fig.8.DMA results for fully cured prepreg during cooling from themaximum temperature,at a cooling rate of 1 K/min.14小结：1.研究聚合物的固化与交联1、观察玻璃化转变，测定玻璃化转变温度2

11、、损耗峰的频率依赖性3、辅助交联过程的分析152.表征材料的阻尼性能Method to characterize the damping behavior of thin passively constrained layer laminates using dynamic mechanical analysis(DMA)in shear mode.文献二162.表征材料的阻尼性能Fig.9.Results of the DMA experiments with the mechanical loss factor tan d as a function of the temperature

12、T for frequencies of 1,10,100 and 200 Hz for laminates a)A.1 and b)A.2.17Knapp G,Oreski G,Pinter G.Method to characterize the damping behavior of thin passively constrained layer laminates using dynamic mechanical analysis(DMA)in shear modeJ.Polymer Testing,2015,42.2.表征材料的阻尼性能Fig.10.Results of the D

13、MA experiments with the mechanical loss factor tan d as a function of the temperature T for frequencies of 1,10,100 and 200 Hz for laminates a)B.1 and b)B.3.18Knapp G,Oreski G,Pinter G.Method to characterize the damping behavior of thin passively constrained layer laminates using dynamic mechanical

14、analysis(DMA)in shear modeJ.Polymer Testing,2015,42.2.表征材料的阻尼性能Fig.11.Results of the DMA experiments with the mechanical loss factor tan d as a function of the temperature T for frequencies of 1,10,100 and 200 Hz for laminate C.1.19Knapp G,Oreski G,Pinter G.Method to characterize the damping behavio

15、r of thin passively constrained layer laminates using dynamic mechanical analysis(DMA)in shear modeJ.Polymer Testing,2015,42.2.表征材料的阻尼性能阻尼性能的评价为了增加数据可比性，用下面的公式求出平均的损耗因子20Knapp G,Oreski G,Pinter G.Method to characterize the damping behavior of thin passively constrained layer laminates using dynamic

16、mechanical analysis(DMA)in shear modeJ.Polymer Testing,2015,42.3.研究聚合物材料的老化性文献三Investigation of accelerated aging behaviour of high performance industrial coatings by dynamic mechanical analysis涂层 A(经济型脂肪族聚氨酯)涂层 B(醇酸改性聚氨酯)涂层 C(高性能脂肪族聚氨酯)涂层 D(脂肪族环氧改性聚硅氧烷)材料A,B,C所用固化剂HDID所用的固化剂：21Mitra S,Ahire A,Malli

17、k B P.Investigation of accelerated aging behaviour of high performance industrial coatings by dynamic mechanical analysisJ.Progress in Organic Coatings,2014,77:18161825.3.研究聚合物材料的老化性DMA测定玻璃化转变温度固化7天后Fig.12.Tan vs.temperature plots of four topcoats.测量模式膜张力模式3K/min 1Hz 0.1应变振幅样品尺寸：2.5CM*0.6CM22Mitra S

18、,Ahire A,Mallik B P.Investigation of accelerated aging behaviour of high performance industrial coatings by dynamic mechanical analysisJ.Progress in Organic Coatings,2014,77:18161825.3.研究聚合物材料的老化性DMA测定玻璃化转变温度固化7天后Fig.13.Glass transition temperatures(T g)of topcoats as obtained from DMA.所有的四款涂料在室温下都是

19、可用的。A涂层的玻璃化转变温度最低，D涂层的玻璃化转变温度最高。23Mitra S,Ahire A,Mallik B P.Investigation of accelerated aging behaviour of high performance industrial coatings by dynamic mechanical analysisJ.Progress in Organic Coatings,2014,77:18161825.3.研究聚合物材料的老化性通过DMA 确定交联密度 通过橡胶平台区的储能模量.用粘弹理论,T为开尔文温度G为剪切模量V=0.5(不可压缩假设)在低频率下

20、用储能模量代替上式中的弹性模量24Mitra S,Ahire A,Mallik B P.Investigation of accelerated aging behaviour of high performance industrial coatings by dynamic mechanical analysisJ.Progress in Organic Coatings,2014,77:18161825.3.研究聚合物材料的老化性通过DMA 确定交联密度 Table 2Various physical parameters as obtained from DMA and calcula

21、ted using Eq.Fig.14.Storage modulus(E)vs.temperature plot of four topcoats25Mitra S,Ahire A,Mallik B P.Investigation of accelerated aging behaviour of high performance industrial coatings by dynamic mechanical analysisJ.Progress in Organic Coatings,2014,77:18161825.B交联密度最小3.研究聚合物材料的老化性分别对上述四种涂层进行老化处

22、理 cyclic-corrosion and UV-B exposure在老化之在老化之后可以看后可以看到到tan.峰峰发生明显发生明显的高温移的高温移动动,同时峰同时峰值下降，值下降，峰形拓宽峰形拓宽 Fig.15.Tan vs.temperature plots before exposure(solid line),after cyclic corrosion(dash-)and after UV-B weathering(dash-dot-dot)showing(a)Coating A,(b)CoatingB,(c)Coating C,and(d)Coating D.26C的性能保的性

23、能保存得最好存得最好3.研究聚合物材料的老化性Fig.16.Tg of topcoats as obtained from DMA before and after cyclic corrosion and UV-B weathering.27Mitra S,Ahire A,Mallik B P.Investigation of accelerated aging behaviour of high performance industrial coatings by dynamic mechanical analysisJ.Progress in Organic Coatings,2014,

24、77:18161825.Fig.17.Crosslink density values all four topcoats before and after cyclic corrosionand UV-B weathering.老化处理后变硬，变脆，玻璃化转变温度升高，交联密度升高，老化处理后变硬，变脆，玻璃化转变温度升高，交联密度升高，分子量降低分子量降低小结 DMA 的应用方面：1、测玻璃化转变温度 2、损耗模量，储能模量，损耗因子 3、阻尼性能的表征 4、老化性能的表征 5、辅助研究固化过程 6、观察多重转变，结晶性等 28参考文献Stark W,Jaunich M.Investiga

25、tion of Ethylene/Vinyl Acetate Copolymer(EVA)by thermal analysis DSC and DMAJ.Polymer Testing,2011,30(2):236-242.Stark W.Investigation of the curing behaviour of carbon fibre epoxy prepreg by Dynamic Mechanical Analysis DMAJ.Polymer Testing,2013,32(2):231239.Mitra S,Ahire A,Mallik B P.Investigation

26、of accelerated aging behaviour of high performance industrial coatings by dynamic mechanical analysisJ.Progress in Organic Coatings,2014,77:18161825.Knapp G,Oreski G,Pinter G.Method to characterize the damping behavior of thin passively constrained layer laminates using dynamic mechanical analysis(DMA)in shear modeJ.Polymer Testing,2015,42.123429谢谢30