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Crosslinking characterization of a polyimide: AFR700B

机译:聚酰亚胺的交联表征:AFR700B

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Crosslinking in AFR700B polyimide was studied using several techniques. Crosslinking could not be detected using Fourier transform infrared spectroscopy (FTIR) and differential scanning calorimetry (DSC). Swelling in n-methyl pyrroli done [NMP) showed network formation occurs at cure temperatures greater than or equal to 325 degrees C (617 degrees F), but the reaction kinetics could not be determined from the data. Dynamic mechanical analysis [DMA] studies have shown that the storage modulus (G') increased with increasing cure temperature up to 350 degrees C (662 degrees F), and was constant above 350 degrees C (662 degrees F), indicating that crosslinking via the reverse Diels-Alder reaction was occurring. A broad secondary transition was seen in the loss modulus (G '') curves, centered between 150 and 180 degrees C (302 and 356 degrees F). This secondary transition appeared at a cure temperature of 300 degrees C (572 degrees F) and became more dominant with increasing temperature and time. This secondary transition was not seen for cures <300 degrees C (572 degrees F) when the chains have not crosslinked. Therefore, this is likely due to a crosslink bond rather than one in the backbone. At 1 atm, crosslinking followed second-order kinetics based on the increase in glass transition temperature (T-g). The Arrhenius plot of the rate constant showed a break in the slope, possibly indicating a change in reaction mechanism. At 1.38 MPa (200 psi), the T-g data was too scattered to determine the kinetics.
机译:使用多种技术研究了AFR700B聚酰亚胺中的交联。使用傅立叶变换红外光谱(FTIR)和差示扫描量热法(DSC)无法检测到交联。在n-甲基吡咯中完成的溶胀[NMP]显示,在大于或等于325摄氏度(617华氏度)的固化温度下会形成网状结构,但无法根据数据确定反应动力学。动态力学分析[DMA]研究表明,储能模量(G')随固化温度的升高而提高,直至350摄氏度(662华氏度),并且在350摄氏度(662华氏度)以上保持恒定,表明通过发生了逆Diels-Alder反应。在损耗模量(G)曲线中看到了一个宽泛的二次跃迁,中心在150到180摄氏度(302和356华氏度)之间。二次转变出现在300摄氏度(572华氏度)的固化温度下,并随着温度和时间的增加而变得更加明显。当链未交联时,对于<300摄氏度(572华氏度)的固化,看不到这种二次过渡。因此,这可能是由于交联键而不是主链中的一个。在1个大气压下,基于玻璃化转变温度(T-g)的增加,交联遵循二级动力学。速率常数的Arrhenius图显示了斜率的折断,可能表明反应机理发生了变化。在1.38 MPa(200 psi)下,T-g数据过于分散,无法确定动力学。

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