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聚酰亞胺-b-聚脲共聚物薄膜的制備研究

發(fā)布時間:2018-04-25 09:23

  本文選題:聚酰亞胺 + 聚脲; 參考:《大連理工大學(xué)》2016年碩士論文


【摘要】:聚酰亞胺(PI)因其優(yōu)異的熱穩(wěn)定性、力學(xué)性能、電性能以及化學(xué)穩(wěn)定性被廣泛應(yīng)用于航空航天、電子電氣、機械、化工等高新技術(shù)領(lǐng)域。隨著科學(xué)技術(shù)的蓬勃發(fā)展,微電子行業(yè)對聚酰亞胺材料的吸水性能提出了更高的要求,傳統(tǒng)的芳香族聚酰亞胺材料已經(jīng)不能滿足微電子行業(yè)不斷發(fā)展的要求。因此,開發(fā)新型低吸水率聚酰亞胺材料具有十分重要的意義。眾所周知,聚脲(PUA)的力學(xué)性能和熱穩(wěn)定性較好,且吸水率較低,若將其與聚酰亞胺共聚,有望在保持聚酰亞胺本身優(yōu)異性能的前提下,降低聚酰亞胺的吸水率。本課題通過溶液聚合的方法合成了聚酰亞胺-b-聚脲(PUI)共聚物。具體方法為:將酸酐終止的聚酰胺酸(PAA)溶液與異氰酸酯終止的聚脲溶液混合,加入交聯(lián)劑進行交聯(lián)反應(yīng),之后經(jīng)過熱亞胺化處理制備了PUI共聚物薄膜,并對該薄膜的性能進行了研究。主要研究內(nèi)容如下:首先,以均苯四甲酸二酐(PMDA)和4,4’-二氨基二苯醚(ODA)為單體,在N-甲基吡咯烷酮(NMP)溶劑中進行溶液聚合,制備酸酐終止的聚酰胺酸溶液,并探究單體配比、加料順序、反應(yīng)溫度、反應(yīng)時間、反應(yīng)物總固含量對聚酰胺酸特性粘數(shù)的影響;其次,以二苯基甲烷-4,4'-二異氰酸酯(MDI)和ODA為單體,在NMP溶劑中進行溶液聚合,制備異氰酸酯終止的聚脲預(yù)聚體溶液;第三,將聚酰胺酸溶液與不同含量的聚脲溶液混合,再加入一定量的ODA進行交聯(lián),然后通過亞胺化處理得到PUI共聚物薄膜。最后,通過FTIR、XRD、SEM、TGA分析對PUI薄膜進行表征,探究了聚脲的含量對PUI接觸角和吸水率的影響。研究發(fā)現(xiàn),制備的PUI共聚物薄膜具有良好的疏水性能,并且隨著聚脲含量的增大,PUI共聚物的接觸角越大、吸水率越低。當聚脲的含量為50mol%時,PUI共聚物薄膜的接觸角為101.56°,吸水率為1.16%。另外,PUI的熱穩(wěn)定性較好,其熱分解溫度在240~245℃之間。
[Abstract]:Polyimide (Pi) has been widely used in aerospace, electronic and electrical, mechanical, chemical and other high-tech fields due to its excellent thermal stability, mechanical properties, electrical properties and chemical stability. With the rapid development of science and technology, the microelectronics industry has put forward higher requirements for the absorbability of polyimide materials. Traditional aromatic polyimide materials can not meet the requirements of the development of the microelectronics industry. Therefore, it is of great significance to develop new low water absorption polyimide materials. It is well known that the mechanical properties and thermal stability of polyurea (PUAA) are good, and the water absorption is low. If copolymerized with polyimide, it is expected to reduce the water absorption of polyimide on the premise of keeping the excellent performance of polyimide itself. In this paper, polyimide-b-polyurea (PUI) copolymers were synthesized by solution polymerization. The specific methods are as follows: the polyamide acid acid (PAA) solution terminated by anhydride is mixed with the polyurea solution terminated by isocyanate, crosslinking reaction is carried out by adding crosslinking agent, and then the PUI copolymer film is prepared by thermal imidization. The properties of the films were also studied. The main research contents are as follows: firstly, the polyamide acid solution terminated by acid anhydride was prepared by solution polymerization in N-methylpyrrolidone (NMPP) solvent with PMDAs and ODAs as monomers, and the monomer ratio was investigated. The effects of feeding order, reaction temperature, reaction time and total solid content of reactants on the intrinsic viscosity of polyamide acid were studied. Secondly, the solution polymerization was carried out in NMP solvent with diphenyl methane-4 (4) -diisocyanate diisocyanate (MDI) and ODA as monomers. The polyurea prepolymer solution terminated by isocyanate was prepared. Thirdly, the polyamide acid solution was mixed with the polyurea solution with different content, then crosslinked with a certain amount of ODA, then the PUI copolymer film was prepared by imidiation. Finally, the PUI films were characterized by FTIR TGA, and the effects of polyurea content on the contact angle and water absorption of PUI were investigated. It is found that the prepared PUI copolymer films have good hydrophobicity, and with the increase of polyurea content, the higher the contact angle of the copolymers, the lower the water absorption. When the content of polyurea is 50 mol%, the contact angle is 101.56 擄and the water absorption is 1.16 擄. In addition, the thermal stability of PUI is better, and its thermal decomposition temperature is between 240 鈩,

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