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Novel acetylene-terminated polyimide oligomers with excellent processability and high toughness of films

机译:新型乙炔封端的聚酰亚胺低聚物,具有优异的可加工性和薄膜高韧性

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A series of acetylene-terminated imide oligomers based on 2,3,3,4-Diphenyl ether tetracarboxylic acid dianhydride (a-ODPA), 3,4-Oxydianiline (3,4-ODA), and 3-Ethynylaniline (3-EA) with different molecular weights were synthesized by using acetic anhydride and triethylamine as dehydrating agent. Their main structure was confirmed by Fourier transform infrared spectroscopy (FT-IR). Thermal curing processing was characterized by FT-IR and differential scanning calorimetry (DSC). All the uncured imide oligomers showed excellent solubility (more than 30 wt %) in organic solvent such as N,N-dimethylacetamide (DMAc) and N-methyl-2-pyrrolidone (NMP). These imide oligomers also possessed a very low viscosity, thus provided better processing window. These oligomers were formulated into thermosetting films by thermal crosslinking of the ethynyl groups. The properties of cured films were evaluated by dynamic mechanical thermal analysis (DMA), thermogravimetric analysis (TGA), and tensile measurement. The glass transition temperature (T-g) and elongation at break of the cured films were found to be almost >260 degrees C and >9.2%, respectively. The cured films in air resulted in higher thermal stability than those under N-2 atmosphere. Experimental results suggested that the introduction of asymmetric and flexible ether-hinge with 3-EA in polyimide oligomers can improve the processability of the imide oligomers and the toughness for a cured sample without sacrificing their thermal-oxidative stability. (c) 2015 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015, 132, 42537.
机译:基于2,3,3,4-二苯醚四羧酸二酐(a-ODPA),3,4-羟二苯胺(3,4-ODA)和3-乙炔基苯胺(3-EA)的一系列乙炔封端的酰亚胺低聚物以乙酸酐和三乙胺为脱水剂合成了不同分子量的二甲基亚砜。它们的主要结构已通过傅里叶变换红外光谱(FT-IR)确认。通过FT-IR和差示扫描量热法(DSC)对热固化过程进行了表征。所有未固化的酰亚胺低聚物均在有机溶剂(例如N,N-二甲基乙酰胺(DMAc)和N-甲基-2-吡咯烷酮(NMP))中显示出极好的溶解度(大于30 wt%)。这些酰亚胺低聚物还具有非常低的粘度,因此提供了更好的加工窗口。通过乙炔基的热交联将这些低聚物配制成热固性膜。通过动态机械热分析(DMA),热重分析(TGA)和拉伸测量来评估固化膜的性能。发现固化膜的玻璃化转变温度(T-g)和断裂伸长率分别分别接近> 260℃和> 9.2%。空气中的固化膜比N-2气氛下的固化膜具有更高的热稳定性。实验结果表明,在聚酰亚胺低聚物中引入带有3-EA的不对称和柔性醚铰链可以改善酰亚胺低聚物的加工性能和固化样品的韧性,而不会牺牲其热氧化稳定性。 (c)2015 Wiley Periodicals,Inc. J. Appl。 Polym。科学2015,132,42537。

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