关键词: dielectric analysis (DEA) dynamic mechanical analysis (DMA) epoxy molding compound (EMC) glass transition temperature (Tg) heterogeneity monitoring response surface

来  源:   DOI:10.3390/polym16111540   PDF(Pubmed)

Abstract:
The in-line control of curing during the molding process significantly improves product quality and ensures the reliability of packaging materials with the required thermo-mechanical and adhesion properties. The choice of the morphological and thermo-mechanical properties of the molded material, and the accuracy of their determination through carefully selected thermo-analytical methods, play a crucial role in the qualitative prediction of trends in packaging product properties as process parameters are varied. This work aimed to verify the quality of the models and their validation using a highly filled molding resin with an identical chemical composition but 10 wt% difference in silica particles (SPs). Morphological and mechanical material properties were determined by dielectric analysis (DEA), differential scanning calorimetry (DSC), warpage analysis and dynamic mechanical analysis (DMA). The effects of temperature and injection speed on the morphological properties were analyzed through the design of experiments (DoE) and illustrated by response surface plots. A comprehensive approach to monitor the evolution of ionic viscosity (IV), residual enthalpy (dHrest), glass transition temperature (Tg), and storage modulus (E) as a function of the transfer-mold process parameters and post-mold-cure (PMC) conditions of the material was established. The reliability of Tg estimation was tested using two methods: warpage analysis and DMA. The noticeable deterioration in the quality of the analytical signal for highly filled materials at high cure rates is discussed. Controlling the temperature by increasing the injection speed leads to the formation of a polymer network with a lower Tg and an increased storage modulus, indicating a lower density and a more heterogeneous structure due to the high heating rate and shear heating effect.
摘要:
在成型过程中对固化的在线控制显着提高了产品质量,并确保了包装材料具有所需的热机械和粘合性能的可靠性。成型材料的形态和热机械性能的选择,以及通过精心选择的热分析方法确定的准确性,随着工艺参数的变化,在包装产品性能趋势的定性预测中起着至关重要的作用。这项工作旨在验证模型的质量和他们的验证使用高度填充的模塑树脂具有相同的化学成分,但在二氧化硅颗粒(SP)的10重量%的差异。通过介电分析(DEA)确定了形态和机械材料性能,差示扫描量热法(DSC),翘曲分析和动态力学分析(DMA)。通过实验设计(DoE)分析了温度和注射速度对形态特性的影响,并通过响应面图进行了说明。一种监测离子粘度(IV)演变的综合方法,残余焓(dHrest),玻璃化转变温度(Tg),和储能模量(E)作为转移模制工艺参数和材料的模制后固化(PMC)条件的函数。使用两种方法测试Tg估计的可靠性:翘曲分析和DMA。讨论了在高固化速率下高度填充材料的分析信号质量的显着下降。通过增加注射速度来控制温度导致形成具有较低Tg和增加的储能模量的聚合物网络,由于高加热速率和剪切加热效应,表明较低的密度和较不均匀的结构。
公众号