RESIDUAL-STRESS BEHAVIOR OF ISOMERIC PMDA-ODA POLYIMIDES
RESIDUAL-STRESS BEHAVIOR OF ISOMERIC PMDA-ODA POLYIMIDES
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DOI：
10.1016/0032-3861(92)90768-r
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发表时间：
1992-01-01
期刊：
影响因子：
4.6
通讯作者：
VOLKSEN, W
中科院分区：
文献类型：
--
作者：
REE, M;NUNES, TL;VOLKSEN, W
聚(3,4'-氧二亚苯基均苯四酰亚胺) (PMDA-3,4'-ODA) 是聚(4,4'-氧二亚苯基均苯四酰亚胺) (PMDA-4,4'-ODA) 的异构体，由均苯四酸二酐 (PMDA) 和 3,4'-氧二亚苯基二胺 (3,4'-ODA) 合成。 对于这两种聚酰亚胺异构体及其在硅晶片上处于凝聚状态的聚酰胺酸前体，通过动态测量晶片弯曲来研究在 25-400 摄氏度范围内的残余应力行为。 在热酰亚胺化过程中，两种异构体在应力与温度行为方面没有表现出任何差异。 然而，一旦酰亚胺化，一种异构体在冷却过程中表现出与另一种异构体完全不同的应力行为：PMDA-3,4'-ODA的应力从400℃时的零快速增加到40℃时几乎等于45MPa，而PMDA-4,4'-ODA的应力从零逐渐上升到几乎等于27MPa。 对于两种固化异构体，加热时的应力-温度曲线与冷却时的应力-温度曲线相同，但由于在 25-150℃ 温度范围内吸湿而存在一些偏差，这表明它们的应力对热循环或热退火不敏感。 根据两种聚酰亚胺独立测量的特性（热膨胀系数、模量、泊松比 0.34），计算热应力并与测量的总应力进行比较。 结论是，对于两种聚酰亚胺，总残余应力主要由热应力产生。 与PMDA-4,4'-ODA相比，PMDA-3,4'-ODA尽管其热膨胀系数略低，但表现出更高的应力。 由此得出结论，异构体应力之间的巨大差异是由于它们的模量差异较大造成的（PMDA-3,4'-ODA 为 5.0 GPa，PMDA-4,4'-ODA 为 3.0 GPa）。 通过广角 X 射线衍射测定，这两种异构体形态结构的差异进一步支持了这种行为：PMDA-3,4'-ODA 显示出发育良好的晶体结构，而 PMDA-4,4'-ODA 则没有。 此外，还研究了聚酰亚胺薄膜和涂有 A1100 底漆的硅片之间的界面粘附力。
Poly(3,4'-oxydiphenylene pyromellitimide) (PMDA-3,4'-ODA), an isomer of poly(4,4'-oxydiphenylene pyromellitimide) (PMDA-4,4'-ODA), was synthesized from pyromellitic dianhydride (PMDA) and 3,4'-oxydiphenylene diamine (3,4'-ODA). For these two polyimide isomers and their poly(amic acid) precursors in the condensed state on Si wafers, residual stress behaviour over the range 25-400-degrees-C was investigated by the dynamic measurement of wafer bending. During thermal imidization both isomers did not show any difference in stress versus temperature behaviour. Once imidized, however, one isomer exhibited a quite different stress behaviour from that of the other during cool-down: the stress of PMDA-3,4'-ODA increased rapidly from zero at 400-degrees-C to almost-equal-to 45 MPa at 40-degrees-C, whereas that of PMDA-4,4'-ODA rose gradually from zero to almost-equal-to 27 MPa. For both cured isomers, stress-temperature profile on heating was the same as that on cooling, with some deviation due to moisture uptake over the temperature range 25-150-degrees-C, indicating that their stresses were insensitive to thermal cycling or thermal annealing. From independently measured properties (thermal expansion coefficient, modulus, Poisson's ratio of 0.34) of both polyimides, the thermal stresses were calculated and compared with the measured overall stresses. It is concluded that for both polyimides the overall residual stress results primarily from the thermal stress. In comparison with PMDA-4,4'-ODA, PMDA-3,4'-ODA showed a much higher stress despite its slightly lower thermal expansion coefficient. This leads to the conclusion that the large difference between the stresses of the isomers results from the large difference in their moduli (5.0 GPa for PMDA-3,4'-ODA and 3.0 GPa for PMDA-4,4'-ODA). This behaviour is further supported by the difference in morphological structures of these two isomers as determined by wide-angle X-ray diffraction: PMDA-3,4'-ODA showed a well-developed crystalline structure, whereas the PMDA-4,4'-ODA did not. In addition, the interfacial adhesion between polyimide film and Si wafer primed with A1100 was investigated.