Microcapsules containing isophorone diisocyanate were fabricated in oil-in-water emulsion. The emulsification effect of different emulsifiers during the capsule synthesis was systematically investigated by optical microscope. Three kinds of shell materials were discussed to obtain the high core content, smooth-surfaced, and robust capsule by scanning electronic microscope and Fourier transform infrared spectroscopy. Self-healing performance of corresponding self-healing epoxy composites was fully evaluated by accelerated corrosion test and mechanical test. The results demonstrated that high core content and smooth-surfaced capsules with dense composite shell could be synthesized in polyvinyl alcohol emulsion, and the core content of the optimized capsules was determined as 71.3–84.6 wt% at the capsule size from 35 µm to 154 µm. In addition, the optimized capsules had good processing properties and the corresponding self-healing epoxy composites exhibited excellent core release and self-healing performance.
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