论文总字数：19050字

摘 要

芳香族聚酰亚胺具有优良的机械性能、高温稳定性、低介电常数、高击穿电压、耐有机溶剂性和易加工等，并在微电子器件、胶片、胶粘剂和薄膜工业等领域中得到了广泛的应用。但随着科学技术的不断发展，原有的聚酰亚胺薄膜越来越难以满足工业应用的要求，故越来越多的研究者投入了PI薄膜的改性，以此来制备或生产出符合要求的PI复合薄膜。本实验则采用相对便宜的疏水性改性剂油酸(OA)对市售纳米二氧化硅(SiO₂)进行表面改性，并通过红外光谱、扫描电镜、热重分析等测试方法对其进行表征。将表面改性后的二氧化硅纳米颗粒(SiO₂-OA)分散在聚酰胺酸(PAA)中，含量从1%-5%，在高温下环化形成一系列PI/SiO₂-OA纳米复合膜(PISA)，随后研究了SiO₂-OA纳米粒子的加入对制备的聚酰亚胺纳米复合材料性能的影响。结果表明，与纯PI和PI/未修饰的SiO₂复合膜(PISI)相比，制备的PISA膜具有更好的热稳定性，并降低了吸水率和热膨胀率。通过此研究制备的PI/SiO₂-OA纳米复合材料在高性能微电子器件中具有广阔的应用前景。

关键词：二氧化硅 纳米颗粒 聚酰亚胺 复合材料 吸水率

The Preparation of Polyimide-Silica Nanocomposites

Abstract

Aromatic polyimides have excellent mechanical properties, high temperature stability, low dielectric constant, high breakdown voltage, resistance to organic solvents and easy processing, etc., and they are widely used in microelectronic devices, film, adhesives and film industry and other fields. However, with the development of science and technology, the original polyimide film is increasingly difficult to meet the requirements of industrial applications, so more and more researchers are engaged in the modification of PI film, in order to prepare or produce PI composite film in line with the requirements.In this study, oleic acid, a relatively inexpensive and hydrophobic modifier, was used to surface-modify a commercially available nano-sized silica(SiO₂) via esteriffication, and the silica was characterized by FTIR, SEM, TGA and the other measurements. The surface-modified silica nanoparticles (SiO₂-OA) were dispersed in a polyamic acid from 1% to 5%, which were then cyclized at high temperature to form a series of PI/SiO₂-OA nanocomposite films(PISA), then the effect of SiO₂-OA nanoparticles on the properties of polyimide nanocomposites was studied. The results indicated that, compared with pure PI and PI/pristine-SiO₂ composite films(PISI), the as-prepared PISA films had enhanced thermal stability, as well as reduced water absorption and thermal expansion. PI/SiO₂-OA nanocomposites prepared through this study have broad application prospects in high-performance microelectronic devices.

Key Words: Silica; Nanoparticles; Polyimide; Composites; Water absorption

目 录

摘要……………………………………………………………………………………………I

ABSTRACT…………………………………………………………………………………II

第一章 文献综述……………………………………………………………………………1

1.1 聚酰亚胺………………………………………………………………………………1

1.1.1 聚酰亚胺简介…………………………………………………………………1

1.1.2 聚酰亚胺的合成方法…………………………………………………………1

1.1.3 聚酰亚胺的性能及用途………………………………………………………2

1.2 聚酰亚胺纳米复合材料………………………………………………………………3

1.2.1 聚酰亚胺改性简介……………………………………………………………3

1.2.2 聚酰亚胺薄膜复合改性填料及方法…………………………………………5

1.2.3 聚酰亚胺纳米复合材料………………………………………………………5

1.3 PI/SiO₂纳米复合材料…………………………………………………………………6

1.4 本课题研究的目的和意义……………………………………………………………7

第二章 实验部分……………………………………………………………………………8

2.1实验仪器与药品………………………………………………………………………8

2.2 样品制备………………………………………………………………………………8

2.2.1 SiO₂-OA纳米粒子的制备……………………………………………………8

2.2.2 聚酰胺酸(PAA)溶液的制备…………………………………………………9

2.2.3 PI/SiO₂-OA纳米复合薄膜的制备……………………………………………9

2.3 表征…………………………………………………………………………………10

第三章 结果与讨论………………………………………………………………………12

3.1 红外光谱……………………………………………………………………………12

3.1.1 SiO₂-OA红外光谱分析……………………………………………………12

3.1.2 PI/SiO₂-OA纳米复合材料红外光谱分析…………………………………13

3.2 扫描电镜……………………………………………………………………………14

3.3 热膨胀系数及玻璃化转变温度……………………………………………………14

3.4 热重分析……………………………………………………………………………15

3.5 吸水率………………………………………………………………………………16

第四章 实验部分…………………………………………………………………………17

4.1 结论…………………………………………………………………………………17

4.2 展望…………………………………………………………………………………17

参考文献……………………………………………………………………………………19

致谢…………………………………………………………………………………………21

1. 文献综述

1.1聚酰亚胺

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