Kim Soohyun, Jang Keon-Soo, Choi Hee-Dok, Choi Seung-Hoon, Kwon Seong-Ji, Kim Il-Doo, Lim Jung Ah, Hong Jae-Min
Energy Institute, Energy and Mineral Engineering, Pennsylvania State University, University Park, PA 16801, USA.
Int J Mol Sci. 2013 Apr 24;14(5):8698-707. doi: 10.3390/ijms14058698.
A wet phase inversion process of polyamic acid (PAA) allowed fabrication of a porous membrane of polyimide (PI) with the combination of a low dielectric constant (1.7) and reasonable mechanical properties (Tensile strain: 8.04%, toughness: 3.4 MJ/m3, tensile stress: 39.17 MPa, and young modulus: 1.13 GPa), with further thermal imidization process of PAA. PAA was simply synthesized from purified pyromellitic dianhydride (PMDA) and 4,4-oxydianiline (ODA) in two different reaction solvents such as γ-butyrolactone (GBL) and N-methyl-2-pyrrolidinone (NMP), which produce Mw/PDI of 630,000/1.45 and 280,000/2.0, respectively. The porous PAA membrane was fabricated by the wet phase inversion process based on a solvent/non-solvent system via tailored composition between GBL and NMP. The porosity of PI, indicative of a low electric constant, decreased with increasing concentration of GBL, which was caused by sponge-like formation. However, due to interplay between the low electric constant (structural formation) and the mechanical properties, GBL was employed for further exploration, using toluene and acetone vs. DI-water as a coagulation media. Non-solvents influenced determination of the PAA membrane size and porosity. With this approach, insight into the interplay between dielectric properties and mechanical properties will inform a wide range of potential low-k material applications.
聚酰胺酸(PAA)的湿法相转化过程能够制备具有低介电常数(1.7)和合理机械性能(拉伸应变:8.04%,韧性:3.4 MJ/m³,拉伸应力:39.17 MPa,杨氏模量:1.13 GPa)的聚酰亚胺(PI)多孔膜,这是通过对PAA进行进一步热亚胺化过程实现的。PAA由纯化的均苯四甲酸二酐(PMDA)和4,4'-二氨基二苯醚(ODA)在两种不同的反应溶剂(如γ-丁内酯(GBL)和N-甲基-2-吡咯烷酮(NMP))中简单合成,分别得到分子量/多分散指数为630,000/1.45和280,000/2.0的产物。多孔PAA膜通过基于GBL和NMP之间特定组成的溶剂/非溶剂体系的湿法相转化过程制备。PI的孔隙率(低介电常数的指标)随着GBL浓度的增加而降低,这是由海绵状结构的形成导致的。然而,由于低介电常数(结构形成)和机械性能之间的相互作用,采用GBL进行进一步探索,使用甲苯和丙酮与去离子水作为凝固介质。非溶剂影响PAA膜尺寸和孔隙率的测定。通过这种方法,深入了解介电性能和机械性能之间的相互作用将为广泛的潜在低k材料应用提供依据。