scholarly journals Effect of Microcapsule Content on Diels-Alder Room Temperature Self-Healing Thermosets

Polymers ◽  
2020 ◽  
Vol 12 (12) ◽  
pp. 3064
Author(s):  
Sadella C. Santos ◽  
John J. La Scala ◽  
Giuseppe R. Palmese

A furan functionalized epoxy-amine thermoset with an embedded microcapsule healing system that utilizes reversible Diels-Alder healing chemistry was used to investigate the influence of microcapsule loading on healing efficiency. A urea-formaldehyde encapsulation technique was used to create capsules with an average diameter of 150 µm that were filled with a reactive solution of bismaleimide in phenyl acetate. It was found that optimum healing of the thermoset occurred at 10 wt% microcapsule content for the compositions investigated. The diffusion of solvent through the crack interface and within fractured samples was investigated using analytical diffusion models. The decrease in healing efficiency at higher microcapsule loading was attributed partially to solvent-induced plasticization at the interface. The diffusion analysis also showed that the 10% optimum microcapsule concentration occurs for systems with the same interfacial solvent concentration. This suggests that additional physical and chemical phenomena are also responsible for the observed optimum. Such phenomena could include a reduction in surface area available for healing and the saturation of interfacial furan moieties by reaction with increasing amounts of maleimide. Both would result from increased microcapsule loading.

2013 ◽  
Vol 07 (03) ◽  
pp. 1350014 ◽  
Author(s):  
BIQIN DONG ◽  
NINGXU HAN ◽  
MING ZHANG ◽  
XIANFENG WANG ◽  
HONGZHI CUI ◽  
...  

In the study, a novel microcapsule technology based self-healing system for concrete structures has been developed. Through situ-polymerization reaction, the microcapsule is formed by urea formaldehyde resin to pack the epoxy material, which is applied to cementitious composite to achieve self-healing effect. The experimental results revealed that the self-healing efficiency of the composite can be accessed from the recovery of the permeability and strength for the cracked cementitious specimens as the healing agent in the microcapsule acting on the cracks directly. Scanning electronic microscope (SEM/EDX) results show that the epoxy resin is released along with the cracking of the cementitious composite and prevent from cracks continued growth. Further studies show that the self-healing efficiency is affected by the pre-loading of composite, particle size of microcapsule, aging duration of healing agent and so on.


2016 ◽  
Vol 7 (47) ◽  
pp. 7278-7286 ◽  
Author(s):  
Jian Zhao ◽  
Rui Xu ◽  
Gaoxing Luo ◽  
Jun Wu ◽  
Hesheng Xia

The poly(siloxane-urethane) elastomers with microphase separation structure and Diels–Alder bonds show high healing efficiency, good mechanical property and good biocompatibility.


2010 ◽  
Vol 143-144 ◽  
pp. 353-357
Author(s):  
Ting Ting Li ◽  
Xing Liu ◽  
Rui Wang

Healing agents significantly affect the efficiency of healing microcracks, which produced from life-time service in composites. And microencapsulating 5-ethylidene-2-norbornene (ENB) with Melamine-Urea-Formaldehyde (MUF) shell possessing higher self-healing efficiency is sensitive to the manufacture temperature profile which is difficult to control but crucial to the microcapsule performance and thus the reproducibility. In this paper, we studied the relationship between heating curve (rate, steps and time) and microcapsule performance (surface morphology, thermal stability and shell thickness). It shows that fast-slower heating stage produces the best quality of microcapsule with proper outer and inner surface which can endure 285°C, and the particle size is about 100m with 400-700nm shell thickness.


Polymers ◽  
2020 ◽  
Vol 12 (9) ◽  
pp. 1918 ◽  
Author(s):  
Hyeong-Jun Jeoung ◽  
Kun Won Kim ◽  
Yong Jun Chang ◽  
Yong Chae Jung ◽  
Hyunchul Ku ◽  
...  

The mechanically-enhanced urea-formaldehyde (UF) microcapsules are developed through a multi-step in situ polymerization method. Optical microscope (OM) and field emission scanning electron microscope (FE-SEM) prove that the microcapsules, 147.4 μm in diameter with a shell thickness of 600 nm, are well-formed. From 1H-nuclear magnetic resonance (1H-NMR) analysis, we found that dicyclopentadiene (DCPD), a self-healing agent encapsulated by the microcapsules, occupies ca. 40.3 %(v/v) of the internal volume of a single capsule. These microcapsules are mixed with EPDM (ethylene-propylene-diene-monomer) and Grubbs’ catalyst via a solution mixing method, and universal testing machine (UTM) tests show that the composites with mechanically-enhanced microcapsules has ca. 47% higher toughness than the composites with conventionally prepared UF microcapsules, which is attributed to the improved mechanical stability of the microcapsule. When the EPDM/microcapsule rubber composites are notched, Fourier-transform infrared (FT-IR) spectroscopy shows that DCPD leaks from the broken microcapsule to the damaged site and flows to fill the notched valley, and self-heals as it is cured by Grubbs’ catalyst. The self-healing efficiency depends on the capsule concentration in the EPDM matrix. However, the self-healed EPDM/microcapsule rubber composite with over 15 wt% microcapsule shows an almost full recovery of the mechanical strength and 100% healing efficiency.


2008 ◽  
Vol 47-50 ◽  
pp. 282-285 ◽  
Author(s):  
Tao Yin ◽  
Min Zhi Rong ◽  
Ming Qiu Zhang

To provide epoxy based composites with self-healing ability, two-component healing system consisting of urea-formaldehyde walled microcapsules containing epoxy (30~70µm in diameter) and CuBr2(2-MeIm)4 (the complex of CuBr2 and 2-methylimidazole) latent hardener was synthesized. When cracks were initiated or propagated in the composites, the neighbor micro-encapsulated epoxy would be damaged and released. As the latent hardener is soluble in epoxy, it can be well dispersed in epoxy composites during composites manufacturing, and hence activate the released epoxy wherever it is. As a result, repair of the cracked sites is completed through curing of the released epoxy. The present work indicated that the plain weave glass fabric laminates using the above self-healing epoxy as the matrix have been provided with self-healing capability.


2020 ◽  
Vol 10 (17) ◽  
pp. 5739
Author(s):  
Xenia Tsilimigkra ◽  
Dimitrios Bekas ◽  
Maria Kosarli ◽  
Stavros Tsantzalis ◽  
Alkiviadis Paipetis ◽  
...  

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.


2021 ◽  
Author(s):  
Alejandra Durand-Silva ◽  
Karen Cortés-Guzmán ◽  
Rebecca Johnson ◽  
Sachini Perera ◽  
Ron Smaldone

Dynamic covalent bonds impart new properties to 3D printable materials that help to establish 3D printing as an accessible and efficient manufacturing technique. Here, we studied the effect of a thermally reversible Diels-Alder crosslinker on the shape stability of photoprintable resins and their self-healing properties. Resins containing different concentrations of dynamic covalent crosslinks in a polyacrylate network showed that the content of dynamic crosslinks plays a key role in balancing shape stability with self-healing ability. The shape stability of the printed objects was evaluated by measuring the dimensional changes after thermal treatment. The self-healing efficiency of the 3D printed resins was characterized with a scratch test and tensile testing. A dynamic covalent crosslink concentration of 1.8 mol % was enough to provide 99% self-healing efficiency without disrupting the shape stability of the printed objects. Our work shows the potential of dynamic covalent bonds in broadening the availability of 3D printable materials that are compatible with vat photopolymerization.


2021 ◽  
Author(s):  
Alejandra Durand-Silva ◽  
Karen Cortés-Guzmán ◽  
Rebecca Johnson ◽  
Sachini Perera ◽  
Ron Smaldone

Dynamic covalent bonds impart new properties to 3D printable materials that help to establish 3D printing as an accessible and efficient manufacturing technique. Here, we studied the effect of a thermally reversible Diels-Alder crosslinker on the shape stability of photoprintable resins and their self-healing properties. Resins containing different concentrations of dynamic covalent crosslinks in a polyacrylate network showed that the content of dynamic crosslinks plays a key role in balancing shape stability with self-healing ability. The shape stability of the printed objects was evaluated by measuring the dimensional changes after thermal treatment. The self-healing efficiency of the 3D printed resins was characterized with a scratch test and tensile testing. A dynamic covalent crosslink concentration of 1.8 mol % was enough to provide 99% self-healing efficiency without disrupting the shape stability of the printed objects. Our work shows the potential of dynamic covalent bonds in broadening the availability of 3D printable materials that are compatible with vat photopolymerization.


2021 ◽  
Author(s):  
Mohd Shamsul Farid Samsudin ◽  
Norfarah Diana Aba ◽  
Muzdalifah Zakaria ◽  
Azmi Mohammed Nor ◽  
Russell Varley ◽  
...  

Abstract Polymer coatings, especially epoxy and polyurethane paint systems, have been widely used to prevent corrosion of metallic components and structures. However, due to environmental and mechanical effects, the barrier efficiency of the coatings may be substantially compromised during transportation and service, as demonstrated by localized scratches, delamination, or stress-related microcracks. Application of a self-healing coating that can restore damages and recover its performance with minimal external intervention could prevent corrosion at the damaged coating. In this present work, the healing efficiency and long-term durability of Boronic Ester (BE) blended with Polyurethane (PU) as a self-healing system for top side coating of offshore platform structures was investigated. The BE was mixed at a ratio of 50:50 with PU resin and applied as a top layer on a PU coated steel plate with a thickness of approximately 300-350 μm. The healing efficiency, mechanical performance, and durability under simulated environmental conditions such as salt spray and UV were investigated according to the related ASTM standards. As a first step, the electrical impedance spectroscopy (EIS) and 3D profilemeter microscope were used to assess the healing ability of the scratched coating at room temperature and humidity level of 85 %. The mechanical performance of the self-healing coating layer was evaluated using a pull off adhesion test to investigate the compatibility of the self-healing system with the existing commercial PU topcoat system, while a long term 3000 hours salt spray and 4200 hours cyclic UV test were performed to evaluate the self-healing coating's durability in harsh conditions. Preliminary assessment using EIS and 3D profilemeter microscopes on the scratched PU/BE self-healing coating revealed significant healing efficiency of more than 80% for healing condition at ambient temperature and humidity level of 85%. The self-healing coating layer also demonstrated excellent adhesion efficiency, with adhesion greater than 300 psi suggesting good compatibility of the BE-PU layer with commercial PU coating. The salt spray and cyclic UV tests that were performed to determine the durability of the self-healing coating revealed that the 50BE/50PU layer remained intact and exhibited good healing performance with more than 80% efficiency even after exposure to harsh conditions. The findings from the study demonstrated that the BE/PU material has the potential to be used as a self-healing system for topside coating of offshore platforms structures, thereby lowering maintenance costs.


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