Linseed oil undergoes an oxidative drying reaction upon exposure to air, resulting in a soft film. The reaction conversion after 48 h reached 88% and 59% when it reacted at room temperature and −20 °C, respectively. Linseed-oil-loaded microcapsules were prepared using a urea-formaldehyde polymer as the shell wall material. The microcapsules were integrated into a commercially available protective coating formulation to prepare self-healing coating formulations with different capsule loadings. The coating formulations were applied on mortar specimens to prepare self-healing coatings. The effect of capsule loading on adhesion strength of the self-healing coating was studied. The self-healing function of the coating was investigated by SEM, a water sorptivity test and an accelerated carbonation test. Successful self-healing was demonstrated for both scratch and crack damage in the coatings. Low-temperature self-healing was demonstrated with a saline solution sorptivity test conducted at −20 °C. The linseed-oil-based microcapsule-type self-healing coating system is a promising candidate as a protective coating for cementitious materials.
Low-temperature self-healing capabilities are essential for self-healing materials exposed to cold environments. Although low-temperature self-healing concepts have been proposed, there has been no report of a microcapsule-type low-temperature self-healing system wherein the healing ability was demonstrated at low temperature. In this work, low-temperature self-healing of a microcapsule-type protective coating was demonstrated. This system employed silanol-terminated polydimethylsiloxane (STP) as a healing agent and dibutyltin dilaurate (DD) as a catalyst. STP underwent a condensation reaction at −20 °C in the presence of DD to give a viscoelastic product. The reaction behavior of STP and the viscoelasticity of the reaction product were investigated. STP and DD were separately microencapsulated by in situ polymerization and interfacial polymerization methods, respectively. The STP- and DD-loaded microcapsules were mixed into a commercial enamel paint, and the resulting formulation was applied to glass slides, steel panels, and mortars to prepare self-healing coatings. When the self-healing coatings were damaged at a low temperature (−20 °C), STP and DD were released from broken microcapsules and filled the damaged area. This process was effectively visualized using a fluorescent dye. The self-healing coatings were scratched and subjected to corrosion tests, electrochemical tests, and saline solution permeability tests. The temperature of the self-healing coatings was maintained at −20 °C before and after scratching and during the tests. We successfully demonstrated that the STP/DD-based coating system has good low-temperature self-healing capability.
Polyimide films have conventionally been prepared by thermal imidization of poly(amic acid)s (PAAs). Here we report that the improvement of tensile strength while increasing (or maintaining) film flexibility of polyimide films was accomplished by simple microwave (MW) irradiation of the PAAs. This improvement in mechanical properties can be attributed to the increase in molecular weight of the polyimides by MW irradiation. Our results show that the mechanical properties of polyimide films can be improved by MW irradiation, which is a green approach that requires relatively low MW power, very short irradiation time, and no incorporation of any additional inorganic substance.
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.
Although self-healing protective coatings have been widely studied, systematic research on healing performance of the coating according to damage width has been rare. In addition, there has been rare reports of self-healing of the protective coating having damage width wider than 100 µm. In this study, self-healing performance of a microcapsule type self-healing protective coating on cement mortar was studied for the coating with damage width of 100–300 µm. The effect of capsule-loading (20 wt%, 30 wt% and 40 wt%), capsule size (65-, 102- and 135-µm-mean diameter) and coating thickness (50-, 80- and 100-µm-thick undercoating) on healing efficiency was investigated by water sorptivity test. Accelerated carbonation test, chloride ion penetration test and scanning electron microscope (SEM) study were conducted for the self-healing coating with a 300-µm-wide damage. Healing efficiency of the self-healing coating decreased with increasing damage width. As capsule-loading, capsule size or coating thickness increased, healing efficiency of the self-healing coating increased. Healing efficiency of 76% or higher was achieved using the self-healing coating with a 300-µm-wide scratch. The self-healing coating with a 200-µm-wide crack showed healing efficiency of 70% or higher. The self-healing coating having a 300-µm-wide scratch showed effective protection of the substrate mortar from carbonation and chloride ion penetration, which was supported by SEM study.
A pyromellitic dianhydride (PMDA) and 4,4′-oxydianiline (ODA)-based oligoimide (PMDA-ODA) was synthesized by a one-step procedure using water as a solvent. The PMDA-ODA particles showed excellent partial wetting properties and were stably dispersed in both water and oil phases. A stable dispersion was not obtained with comparison PMDA-ODA particles that were synthesized by a conventional two-step method using an organic solvent. Both oil-in-water and water-in-oil Pickering emulsions were prepared using the oligoimide particles synthesized in water, and the size of the emulsion droplet was controlled based on the oligoimide particle concentration. The oligoimide particles were tested to prepare Pickering emulsions using various kinds of oils. The oil-in-water Pickering emulsions were successfully applied to prepare microcapsules of the emulsion droplets. Our new Pickering emulsion stabilizer has the advantages of easy synthesis, no need for surface modification, and the capability of stabilizing both oil-in-water and water-in-oil emulsions.