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含新制纳米级次磷酸铝(AlPO)的环氧复合材料的固化动力学及热稳定性

Curing Kinetics and Thermal Stability of Epoxy Composites Containing Newly Obtained Nano-Scale Aluminum Hypophosphite (AlPO).

作者信息

Tikhani Farimah, Moghari Shahab, Jouyandeh Maryam, Laoutid Fouad, Vahabi Henri, Saeb Mohammad Reza, Dubois Philippe

机构信息

School of Chemical Engineering, College of Engineering, University of Tehran, Tehran 11155-4563, Iran.

Université de Lorraine, CentraleSupélec, LMOPS, F-57000 Metz, France.

出版信息

Polymers (Basel). 2020 Mar 12;12(3):644. doi: 10.3390/polym12030644.

Abstract

For the first time, nano-scale aluminum hypophosphite (AlPO) was simply obtained in a two-step milling process and applied in preparation of epoxy nanocomposites varying concentration (0.1, 0.3, and 0.5 wt.% based on resin weight). Studying the cure kinetics and thermal stability of these nanocomposites would pave the way toward the design of high-performance nanocomposites for special applications. Scanning electron microscopy (SEM) and transmittance electron microscopy (TEM) revealed AlPO particles having domains less than 60 nm with high potential for agglomeration. (at heating rate of 5 °C/min) and (at heating rates of 10, 15 and 20 °C/min) cure states were detected for nanocomposites under nonisothermal differential scanning calorimetry (DSC). While the dimensionless curing temperature interval () was almost equal for epoxy/AlPO nanocomposites, dimensionless heat release () changed by densification of polymeric network. Quantitative cure analysis based on isoconversional and methods gave rise to the kinetic parameters such as activation energy and the order of reaction as well as frequency factor. Variation of glass transition temperature () was monitored to explain the molecular interaction in the system, where increased from 73.2 °C for neat epoxy to just 79.5 °C for the system containing 0.1 wt.% AlPO. Moreover, thermogravimetric analysis (TGA) showed that nanocomposites were thermally stable.

摘要

首次通过两步研磨工艺简单地制备出了纳米级次磷酸铝(AlPO),并将其应用于制备不同浓度(基于树脂重量分别为0.1、0.3和0.5 wt.%)的环氧纳米复合材料。研究这些纳米复合材料的固化动力学和热稳定性将为特殊应用的高性能纳米复合材料的设计铺平道路。扫描电子显微镜(SEM)和透射电子显微镜(TEM)显示,AlPO颗粒具有小于60 nm的区域,且团聚可能性很高。在非等温差示扫描量热法(DSC)下检测了纳米复合材料的固化状态(加热速率为5℃/min)以及(加热速率为10、15和20℃/min)。虽然环氧/AlPO纳米复合材料的无量纲固化温度区间()几乎相等,但无量纲热释放()随聚合物网络的致密化而变化。基于等转化率和方法的定量固化分析得出了动力学参数,如活化能、反应级数以及频率因子。监测玻璃化转变温度()的变化以解释体系中的分子相互作用,其中,纯环氧树脂的为73.2℃,而含0.1 wt.% AlPO的体系仅为79.5℃。此外,热重分析(TGA)表明纳米复合材料具有热稳定性。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/6089/7183063/5fae36273226/polymers-12-00644-g0A1.jpg

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