On the study of novel self-healing coating: Micro/nano capsule synthesis, coating preparation and property investigation (original) (raw)
Related papers
Preparation and Property Investigation of Epoxy/Amine Micro/Nanocapsule Based Self-healing Coatings
International Polymer Processing, No. 5, 2018
Autonomous self-healing was achieved by synthesizing epoxy coatings which contain dual micro/nanocapsules; epoxy and amine. Epoxy micro/nanocapsules were prepared by an in situ polymerization process and amine microcapsules were fabricated by vacuum infiltration of diethylenetriamine into nanoporous hollow glass microspheres. Both types of capsules were embedded into epoxy matrix. When cracks were created and started to grow in the coating, the micro/nano-capsules near the crack were ruptured and released their contents. As a result of curing reaction between released curing agents (epoxy and amine), healing of the cracked sites was completed. In this work, some properties of epoxy/amine micro/nanocapsule based self-healing coatings such as morphology of micro/nanocapsule and coating, healing and corrosion properties were studied. Also thermal stability and adhesion properties of this kind of coating were evaluated comprehensively. It was found out that optimum mass ratio of epoxy/amine capsules ratio is 1 : 1 and the highest healing efficiency was achieved for a total micro/nanocapsule concentration of 15 wt.%. Regarding thermal and adhesion behavior of coatings, it was observed that adding micro/nano-capsules to epoxy matrix did not change these properties significantly which means self-healing characteristics were achievable without deteriorating other properties.
Journal of Applied Polymer Science, 2019
Silica-polyurea/polyuretane hybrid shell microcapsules (MCs) loaded with isophorone diisocyanate (IPDI) with long shelflife and high thermal and chemical stability are prepared via emulsification followed by interfacial polymerization at the surface of oil droplets of the oil-in-water emulsion. The resultant MCs are aimed at self-healing performance in epoxy coatings. A commercially available, highly reactive polyisocyanate named tris(p-isocyanatophenyl) thiophosphate is successfully employed as shell forming agent, while triethoxyoctylsilane and hexadecyltrimethoxysilane (HDMS) are tested as "latent" active hydrogen sources. The resulting MCs display core-shell morphology, spherical shape with diameter of 5-20 μm, shell thickness ca. 1-2 μm, and an IPDI core fraction of 69 and 65 wt %, when HDMS and triethoxyoctylsilane are employed, respectively. MCs exhibit an increased thermal stability, comparing with pure IPDI, which makes them robust enough to resist the thermal cycles involved in the coating's preparation. Stability of MCs inside specific solvents and chemicals, their chemical composition and shelf-life as well as effect of MCs on the epoxy curing are evaluated by Fourier transformed infrared spectroscopy. MCs, remarkably, show excellent environment stability and a long shelf-life of more than 3.5 months. Their addition to an epoxy formulation is found to heal damaged zones in the epoxy coating, as shown by scanning electron microscopy and electrochemical impedance spectroscopy.
Applications of Microcapsules in Self-Healing Polymeric Materials
Microencapsulation - Processes, Technologies and Industrial Applications [Working Title]
Self-healing polymeric materials have a great potential to be explored and utilized in many applications such as engineering and surface coating. Various smart materials with self-healing ability and unique self-healing mechanisms have been reported in recent publications. Currently, the most widely employed technique is by embedding microcapsules that contain a healing agent into the bulk polymer matrix. When cracks develop in the polymer matrix, the curing agent is released from the microcapsules to cross-link and repair the cracks. Microencapsulation of the healing agent in the core can be achieved by in situ polymerizing of shell material. This chapter presents a general review on self-healing materials, and particularly, self-healing of epoxy matrices that includes epoxy composite and epoxy coating by microencapsulation technique. Microencapsulation processes, including types of resin used, processing parameters such as core/shell ratio, concentration of emulsifiers, viscosities of aqueous and organic phases and stirring rate are discussed.
Robust synthesis of epoxy resin-filled microcapsules for application to self-healing materials
Philosophical transactions. Series A, Mathematical, physical, and engineering sciences, 2016
Mechanically and thermally robust microcapsules containing diglycidyl ether bisphenol A-based epoxy resin and a high-boiling-point organic solvent were synthesized in high yield using in situ polymerization of urea and formaldehyde in an oil-in-water emulsion. Microcapsules were characterized in terms of their size and size distribution, shell surface morphology and thermal resistance to the curing cycles of commercially used epoxy polymers. The size distribution of the capsules and characteristics such as shell thickness can be controlled by the specific parameters of microencapsulation, including concentrations of reagents, stirrer speed and sonication. Selected microcapsules, and separated core and shell materials, were analysed using thermogravimetric analysis and differential scanning calorimetry. It is demonstrated that capsules lose minimal 2.5 wt% at temperatures no higher than 120°C. These microcapsules can be applied to self-healing carbon fibre composite structural materi...
Particuology, 2017
Micro/nanocapsules of urea-formaldehyde resin loaded with linseed oil, which are a self-healing agent in glass flake epoxy anti-corrosion paint, were prepared using a combination of ultrasonic homogenization and in-situ polymerization. The main objective of this study was to model and optimize the microencapsulation process. Five-level central composite design was used to design, model, and optimize the microencapsulation process. A quadratic model was constructed to show the dependency of the percentage of encapsulated linseed oil and capsule size, as model responses, on the studied independent variables (the rotational speed of the agitator and the power and duration of sonication). Analysis of variance showed that all of the variables have significant effects on the encapsulated linseed oil percentage, while the rotational speed of the agitator and sonication time is effective variables for controlling the capsule size. Under the determined optimum conditions, a maximum encapsulated linseed oil percentage (ELO%) of 93.9% and a minimum micro/nanocapsule size of 0.574 m were achieved at 594 rpm agitation, 350 W sonication power, and 3 min sonication time. Validation of the model was performed. The percentage relative errors between the predicted and experimental values of the ELO% and micro/nanocapsule size are 1.28% and 3.66%, respectively. The efficacy of the optimum micro/nanocapsules in healing cracks in a glass flake epoxy paint and corrosion protection was investigated by the salt spray test and Tafel polarization technique.
Polymer Science, Series B, Vol. 59, No. 3, 1–11, 2017
–In the field of coatings, extensive laboratory research has been conducted in the last decade. In the present work, effectiveness of epoxy resin filled micro/nanocapsules was investigated for future using in healing of cracks generated in coatings. Micro/nanocapsules were prepared by in situ polymerization of urea– formaldehyde resin to form shell over epoxy resin droplets. The optimal process parameters for synthesizing the micro/nanocapsules were selected. The as-synthesized capsules were studied by various characterizations techniques, including scanning electron microscope (SEM), particle size analyzer (PSA), Fourier transform-infrared spectroscopy (FTIR), thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC). The results indicate that micro/nanocapsules containing epoxy resins can be synthesized successfully. The rough outer surface of microcapsule is composed of agglomerated urea–formaldehyde nanoparticles. They basically exhibit good storage stability at room temperature, and they are chemically stable before the heating temperature is up to approximately 250°C.
Effect Of TETA Microcapsules On Self-healing Ability Of Dual Component Epoxy System
Advanced Materials Letters, 2016
To deliver epoxy composites with enhanced self-healing ability, this study investigates healing efficiency of dual component epoxy system consisting of microcapsules containing epoxy (DGEBA) and different variants of hardener (TETA) microcapsules. Morphological investigation under FESEM confirms formation of spherical shaped intact TETA microcapsules at high agitation speed with average size of the ~65.32 µm and reduced wall thickness of ~1.823 µm. Reaction temperature is found to play significant role to tune the roughness of the microcapsule surfaces. The single edge notched bending (SENB) test was performed to evaluate the healing ability. It was found that with incorporation of microcapsules, the fracture toughness decreases but the healing efficiency increases with increase in content of microcapsules. The maximum healing efficiency observed was 65.61%. High concentration of TETA microcapsule (prepared at high agitation speed) in epoxy network gives the essence for their applicability as a potential ingredient to elevate the healing efficiency. To enhance the healing ability further of the composites as well as fibre reinforced composites with unaltered mechanical properties we believe synthesis nanocapsules and their incorporation could have significant impact.
Design Strategy for Self-Healing Epoxy Coatings
Coatings, 2020
Self-healing strategies including intrinsic and extrinsic self-healing are commonly used for polymeric materials to restore their appearance and properties upon damage. Unlike intrinsic self-healing tactics where recovery is based on reversible chemical or physical bonds, extrinsic self-healing approaches rely on a secondary phase to acquire the self-healing functionality. Understanding the impacts of the secondary phase on both healing performance and matrix properties is important for rational system design. In this work, self-healing coating systems were prepared by blending a bio-based epoxy from diglycidyl ether of diphenolate esters (DGEDP) with thermoplastic polyurethane (TPU) prepolymers. Such systems exhibit polymerization induced phase separation morphology that controls coating mechanical and healing properties. Structure–property analysis indicates that the degree of phase separation is controlled by tuning the TPU prepolymer molecular weight. Increasing the TPU prepolym...
Curing of epoxy/alkyd blends in self-healing coating
High Performance Polymers, 2018
Self-healing of polymeric material using microcapsules has been developed to repair microcracks within the materials. The self-healing character is reflected from the curing behavior of the material. In this work, curing study of alkyd/epoxy blend was carried out by replacing part of amine hardener with alkyd in the epoxy formulation. The inclusion of alkyd in the epoxy blend resulted in higher degree of curing and higher thermal stability compared to the alkyd-free blend, as evidenced from higher heat of reaction values of differential scanning calorimetry and maximum degradation temperature at 379°C, respectively. Self-healing reaction of epoxy coating as evaluated by Fourier-transform spectroscopy revealed that the 914 cm−1 peak attributed to C–O–C of epoxy has decreased, as the epoxide group was consumed in the reaction. Appearance of a new peak at 1631–1632 cm−1 in the cured coating confirmed that the epoxide has reacted with the carboxylic acid group of alkyd to form ester.
Materials, 2017
A microcapsule-type self-healing protective coating with secondary crack preventing capability has been developed using a silanol-terminated polydimethylsiloxane (STP)/dibutyltin dilaurate (DD) healing agent. STP undergoes condensation reaction in the presence of DD to give a viscoelastic substance. STP-and DD-containing microcapsules were prepared by in-situ polymerization and interfacial polymerization methods, respectively. The microcapsules were characterized by Fourier-transform infrared (FT-IR) spectroscopy, optical microscopy, and scanning electron microscopy (SEM). The microcapsules were integrated into commercial enamel paint or epoxy coating formulations, which were applied on silicon wafers, steel panels, and mortar specimens to make dual-capsule self-healing protective coatings. When the STP/DD-based coating was scratched, self-healing of the damaged region occurred, which was demonstrated by SEM, electrochemical test, and water permeability test. It was also confirmed that secondary crack did not occur in the healed region upon application of vigorous vibration to the self-healing coating.