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Effect of curing history on the residual stress behavior of polyimide thin films

机译：固化历程对聚酰亚胺薄膜残余应力行为的影响

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摘要

The effect of curing history on the residual stress behavior in semiflexible structure poly(4,4 prime -oxydiphenylene pyromellitimide) (PMDA-ODA) and rigid structure poly(p-phenylene biphenyltetracarboximide) (BPDA-PDA) polyimide was investigated. Depending upon the curing history and different structures of polyimide, the residual stress behaviors and the morphology of polyimide thin films were detected in situ by using a wafer bending technique and wide angle X-ray diffraction (WAXD), respectively. For the rigid structure BPDA-PDA polyimide, the residual stress and the slope decreased from 11.7 MPa and 0.058 MPa/°C to 4.2 MPa and 0.007 MPa/°C as the curing temperature increased, and the annealing process is done. However, for the semiflexible structure PMDA-ODA, the change of the residual stress and the slope was relatively not significant. In addition, it was found that the cured polyimide prepared at a higher temperature with a multistep curing process showed a higher order of chain in-plain orientation and packing order than does the polyimide film prepared at a lower temperature with a one-step curing process. These residual stress behaviors of polyimide thin films show good agreement with WAXD results, such as polyimide chain order, orientation, and intermolecular packing order, due to curing history. Specifically, it shows that the effect of curing history on residual stress as well as morphological change was significant in rigid BPDA-PDA polyimide but, not in semiflexible PMDA-ODA polyimide. Therefore, it suggests that the morphological structure depends upon curing history, and the polyimide backbone structure might be one of important factors to lead the low residual stress in polyimide thin films.
机译：研究了固化历史对半柔性结构聚（4,4伯-氧联苯亚均苯四甲酰亚胺）（PMDA-ODA）和刚性结构聚（对亚苯基联苯四碳四酰亚胺）（BPDA-PDA）聚酰亚胺中残余应力行为的影响。根据固化历史和聚酰亚胺的不同结构，分别通过晶片弯曲技术和广角X射线衍射（WAXD）原位检测聚酰亚胺薄膜的残余应力行为和形貌。对于刚性结构的BPDA-PDA聚酰亚胺，随着固化温度的升高，残余应力和斜率从11.7 MPa和0.058 MPa /°C降低到4.2 MPa和0.007 MPa /°C，并进行了退火工艺。但是，对于半柔性结构PMDA-ODA，残余应力和斜率的变化相对不明显。另外，发现在多步骤固化过程中在较高温度下制备的固化的聚酰亚胺与在一步固化过程中在较低温度下制备的聚酰亚胺膜相比，显示出更高的链内取向和堆积顺序。 。由于固化历史，聚酰亚胺薄膜的这些残余应力行为与WAXD结果显示出良好的一致性，例如聚酰亚胺链顺序，取向和分子间堆积顺序。具体来说，它表明固化历史对残余应力以及形态变化的影响在刚性BPDA-PDA聚酰亚胺中很明显，而在半柔性PMDA-ODA聚酰亚胺中则没有。因此，这表明其形态结构取决于固化历史，而聚酰亚胺主链结构可能是导致聚酰亚胺薄膜中残余应力低的重要因素之一。

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