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以4,4’-二氨基二苯硫醚(SDA)和联苯四酸酐(BPDA)为原料,通过溶液缩聚-热酰亚胺化/化学酰亚胺化的方法制备了一种新型的含硫醚结构联苯型聚酰亚胺。利用高级旋转流变仪在线跟踪反应进程,采用热失重分析仪研究反应条件对热酰亚胺化及化学酰亚胺化法的影响,为进一步制备高性能的聚酰亚胺建立有效的实验手段和方法。采用小角激光光散射法、红外光谱、元素分析、接触角仪、DSC等方法对聚合物的结构与性能进行表征。结果显示,硫醚结构的引入使聚合物的表面张力与铜箔相当,可有效改善聚合物薄膜的表面性能,其与铜箔之间的黏附功明显大于传统聚酰亚胺,在无胶挠性线路板应用方面显示出较好的应用前景。所获聚合物的绝对重均相对分子质量为(3.8±1.1)×104g/mol,分解温度均高于560℃;DSC的结果显示所制备的两种酰亚胺化聚合物均具有较高的玻璃化转变温度,相比之下,化学酰亚胺化更有利于获得高酰亚胺化程度的聚合物,产物的玻璃化转变温度也更高。
A new type of polycarboxylic acid with the content of 4,4’-diaminodiphenyl sulfide (SDA) and biphenyltetracarboxylic anhydride (BPDA) was prepared by solution polycondensation-thermal imidization / chemical imidization Sulfide structure Biphenyl polyimide. The progress of the reaction was tracked on-line with a high-grade rotary rheometer, and the influence of reaction conditions on thermal imidization and chemical imidization was investigated by using a thermogravimetric analyzer to establish an effective experimental method for further preparing high-performance polyimide And method. The structures and properties of the polymers were characterized by small-angle laser light scattering, infrared spectroscopy, elemental analysis, contact angle and DSC. The results show that the introduction of sulfide structure makes the surface tension of the polymer equivalent to that of the copper foil, which can effectively improve the surface properties of the polymer film. The adhesion between the copper foil and the polyimide is obviously greater than that of the traditional polyimide. Application of the circuit board shows a good application prospects. The absolute weight average molecular weight of the obtained polymer was (3.8 ± 1.1) × 104g / mol and the decomposition temperature was higher than 560 ℃. The DSC results showed that the prepared two kinds of imidized polymers all had higher Glass transition temperature, in contrast, chemical imidization is more conducive to obtain a high degree of imidization polymer, the glass transition temperature of the product is also higher.