We report the synthesis of controlled sized Urea-formaldehyde (UF) microcapsules containing an epoxy healing agent via in situ emulsification polymerization for the study of self-healing epoxy systems. Scanning Electron Microscopy (SEM) confirmed that the capsules possessed rough external surface which enhanced mechanical interlocking. Differential Scanning Calorimetry (DSC), Thermogravimetric Analysis (TGA) and Solid-state Nuclear Magnetic Resonance (NMR) spectroscopy were employed so as to determine the capsules thermal stability and decompositions and
Microcapsule-based carbon fiber reinforced composites were manufactured by wet layup, in order to assess their mechanical properties and determine their healing efficiency. Microcapsules at 10%wt. containing bisphenol-A epoxy, encapsulated in a urea formaldehyde (UF) shell, were employed with Scandium (III) Triflate (Sc (OTf)3) as the catalyst. The investigation was deployed with two main directions. The first monitored changes to the mechanical performance due to the presence of the healing agent within the composite. More precisely, a minor decrease in interlaminar fracture toughness (GIIC) (−14%), flexural strength (−12%) and modulus (−4%) compared to the reference material was reported. The second direction evaluated the healing efficiency. The experimental results showed significant recovery in fracture toughness up to 84% after the healing process, while flexural strength and modulus healing rates reached up to 14% and 23%, respectively. The Acoustic Emission technique was used to support the experimental results by the onsite monitoring.
In this study, the mechanical properties of purposefully synthesized vitrimer repairable epoxy composites were investigated and compared to conventional, commercial systems. The purpose was to assess the knockdown effect, or the relative property deterioration, from the use of the vitrimer in several testing configurations. Mechanical tests were performed using ILSS, low-velocity impact, and compression after impact configurations. At modeled structure level, the lap strap geometry that can simulate the stiffening of a composite panel was tested. Several non-destructive evaluation techniques were utilized simultaneously with the mechanical testing in order to evaluate (i) the production quality, (ii) the damage during or after mechanical testing, and (iii) the repair efficiency. Results indicated that the new repairable composites had the same mechanical properties as the conventional aerospace-grade RTM6 composites. The electrical resistance change method proved to be a valuable technique for monitoring deformations before the initiation of the debonding and the progress of the damage with consistency and high sensitivity in real time. In terms of repair efficiency, the values ranged from 70% to 100%.
In this study, the effect of the addition of multi-walled carbon nanotubes (MWCNTs), at three percentages, into the urea-formaldehyde (UF) shell-wall of microcapsules on the healing efficiency is reported. The modified shell-wall created a conductive network in semi-conductive epoxies, which led to an improvement of the electromagnetic interference shielding effectiveness (EMI SE); utilizing the excellent electrical properties of the CNTs. The microcapsule’s mean diameter and shell wall were examined via scanning electron microscopy (SEM). Thermal stability was evaluated via thermogravimetric analysis (TGA). The healing efficiency was assessed in terms of fracture toughness, while the electrical properties were measured using impedance spectroscopy. The measurements of the EMI SE were carried out in the frequency range of 7–9 GHz. The derived results indicated that the incorporation of the CNTs resulted in a decrease in the mean size of the microcapsules, while the thermal stability remained unchanged. In particular, the introduction of 0.5% w/v CNTs did not affect the healing efficiency, while it increased the initial mechanical properties of the epoxy after the incorporation of the self-healing system by 27%. At the same time, it led to the formation of a conductive network, providing electrical conductivity to the epoxies. The experimental results showed that the SE increased on average 5 dB or more after introducing conductive microcapsules.
In this work, we report for the first time the manufacturing and characterization of smart multifunctional, capsule-based self-healing and self-sensing composites. In detail, neat and nanomodified UF microcapsules were synthesized and incorporated into composites with a nanomodified epoxy matrix for the restoration of the mechanical and electrical properties. The electrical properties were evaluated with the use of the impedance spectroscopy method. The self-healing composites were subjected to mode-II fracture toughness tests. Additionally, the lap strap geometry that can simulate the mechanical behavior of a stiffened panel was used. The introduction of the nanomodified self-healing system improved the initial mechanical properties in the mode-II fracture toughness by +29%, while the values after the healing process exceeded the initial one. At lap strap geometry, the incorporation of the self-healing system did not affect the initial mechanical properties that were fully recovered after the healing process.
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