Li Danning, Barrington James, James Stephen, Ayre David, Słoma Marcin, Lin Meng-Fang, Yazdani Nezhad Hamed
Enhanced Composites and Structures Centre, School of Aerospace, Transport and Manufacturing, Cranfield University, Cranfield, UK.
Centre for Engineering Photonics, School of Aerospace, Transport and Manufacturing, Cranfield University, Cranfield, UK.
Sci Rep. 2022 May 7;12(1):7504. doi: 10.1038/s41598-022-11380-9.
Failure in an epoxy polymer composite material is prone to initiate by the coalescence of microcracks in its polymer matrix. As such, matrix toughening via addition of a second phase as rigid or/and rubber nano/micro-particles is one of the most popular approaches to improve the fracture toughness across multiple scales in a polymer composite, which dissipates fracture energy via deformation mechanisms and microcracks arrest. Few studies have focused on tailorable and variable toughening, so-called 'active toughening', mainly suggesting thermally induced strains which offer slow and irreversible toughening due to polymer's poor thermal conductivity. The research presented in the current article has developed an instantaneous, reversible extrinsic strain field via remote electromagnetic radiation. Quantification of the extrinsic strain evolving in the composite with the microwave energy has been conducted using in-situ real-time fibre optic sensing. A theoretical constitutive equation correlating the exposure energy to micro-strains has been developed, with its solution validating the experimental data and describing their underlying physics. The research has utilised functionalised dielectric ferroelectric nanomaterials, barium titanate (BaTiO), as a second phase dispersed in an epoxy matrix, able to introduce microscopic electro-strains to their surrounding rigid epoxy subjected to an external electric field (microwaves, herein), as result of their domain walls dipole displacements. Epoxy Araldite LY1564, a diglycidyl ether of bisphenol A associated with the curing agent Aradur 3487 were embedded with the BaTiO nanoparticles. The silane coupling agent for the nanoparticles' surface functionalisation was 3-glycidoxypropyl trimethoxysilane (3-GPS). Hydrogen peroxide (HO, 30%) and acetic acid (CHO, 99.9%) used as functionalisation aids, and the ethanol (CHO, 99.9%) used for BaTiO dispersion. Firstly, the crystal microstructure of the functionalised nanoparticles and the thermal and dielectric properties of the achieved epoxy composite materials have been characterised. It has been observed that the addition of the dielectric nanoparticles has a slight impact on the curing extent of the epoxy. Secondly, the surface-bonded fibre Bragg grating (FBG) sensors have been employed to investigate the real-time variation of strain and temperature in the epoxy composites exposed to microwaves at 2.45 GHz and at different exposure energy. The strains developed due to the in-situ exposure at composite, adhesive and their holding fixture material were evaluated using the FBG. The domain wall induced extrinsic strains were distinguished from the thermally induced strains, and found that the increasing exposure energy has an instantaneously increasing effect on the development of such strains. Post-exposure Raman spectra showed no residual field in the composite indicating no remnant strain field examined under microwave powers < 1000 W, thus suggesting a reversible strain introduction mechanism, i.e. the composite retaining its nominal properties post exposure. The dielectric composite development and quantifications presented in this article proposes a novel active toughening technology for high-performance composite applications in numerous sectors.
环氧聚合物复合材料中的失效往往是由其聚合物基体中的微裂纹合并引发的。因此,通过添加刚性或/和橡胶纳米/微米颗粒等第二相来增韧基体,是提高聚合物复合材料多尺度断裂韧性的最常用方法之一,该方法通过变形机制和微裂纹止裂来耗散断裂能量。很少有研究关注可定制的可变增韧,即所谓的“主动增韧”,主要是指热致应变,由于聚合物的热导率较差,这种应变提供的是缓慢且不可逆的增韧效果。本文所展示的研究通过远程电磁辐射开发出了一种瞬时、可逆的非本征应变场。利用原位实时光纤传感对复合材料中随微波能量演化的非本征应变进行了量化。已经建立了一个将辐照能量与微应变相关联的理论本构方程,其解验证了实验数据并描述了其 underlying 物理原理。该研究使用了功能化的介电铁电纳米材料钛酸钡(BaTiO)作为分散在环氧基体中的第二相,由于其畴壁偶极位移,在外部电场(本文中为微波)作用下,能够在其周围的刚性环氧树脂中引入微观电应变。环氧双酚A二缩水甘油醚Araldite LY1564与固化剂Aradur 3487被用于嵌入BaTiO纳米颗粒。用于纳米颗粒表面功能化的硅烷偶联剂是3 - 缩水甘油氧基丙基三甲氧基硅烷(3 - GPS)。过氧化氢(HO,30%)和乙酸(CHO,99.9%)用作功能化助剂,乙醇(CHO,99.9%)用于BaTiO的分散。首先,对功能化纳米颗粒的晶体微观结构以及所制备的环氧复合材料的热性能和介电性能进行了表征。已经观察到介电纳米颗粒的添加对环氧树脂的固化程度有轻微影响。其次,采用表面粘结的光纤布拉格光栅(FBG)传感器来研究在2.45 GHz微波以及不同辐照能量下暴露于微波的环氧复合材料中应变和温度的实时变化。使用FBG评估了复合材料、粘合剂及其固定夹具材料在原位暴露时产生的应变。区分了畴壁诱导的非本征应变和热致应变,发现增加辐照能量对这种应变的发展有瞬时增加的影响。辐照后的拉曼光谱显示复合材料中没有残余场,这表明在微波功率<1000 W下未检测到残余应变场,从而表明存在一种可逆应变引入机制,即复合材料在辐照后保持其标称性能。本文中所展示的介电复合材料的开发和量化为众多领域的高性能复合材料应用提出了一种新型主动增韧技术。