A process for the microencapsulation of dicyclopentadiene (DCPD) by in situ polymerization of urea-formaldehyde (UF) in an oil-in-water emulsion was developed to meet the requirements for self-healing materials. Microcapsules with average diameters ranging from 10–1000 μm were produced by adjusting the agitation rate between 200–2000 rpm. A linear relationship exists between log(mean diameter) and log(agitation rate). Microcapsules have a smooth inner membrane (160–220 nm) and a rough, porous outer surface composed of agglomerated UF nanoparticles. Surface morphology is influenced by pH and interfacial surface area. High yields (80–90%) of free-flowing spherical microcapsules with fill content of 83–92 wt% were achieved. The microcapsules are robust and suitable for self-healing applications. During microencapsulation, UF nanoparticles form and deposit on the microcapsule surface, creating a rough surface morphology. This roughness enhances mechanical adhesion when embedded in a polymer and improves self-healing performance. However, maintaining constant pH prevents nanoparticle deposition but reduces yields. Increasing the core-water interfacial area produces microcapsules with smooth surfaces and high yields. Fill content remains high for the required time frame for self-healing polymer production. The microcapsules are composed of a UF shell containing DCPD, with excellent storage and release properties. The process provides a unique toughening mechanism for composite systems. The microcapsules are prepared by in situ polymerization in an oil-in-water emulsion, with the reaction conditions carefully controlled to achieve desired microcapsule properties. The microcapsules are analyzed using optical and electron microscopy to determine size, morphology, and shell thickness. The study highlights the importance of process variables in controlling microcapsule size and surface morphology, which are critical for the performance of self-healing materials.A process for the microencapsulation of dicyclopentadiene (DCPD) by in situ polymerization of urea-formaldehyde (UF) in an oil-in-water emulsion was developed to meet the requirements for self-healing materials. Microcapsules with average diameters ranging from 10–1000 μm were produced by adjusting the agitation rate between 200–2000 rpm. A linear relationship exists between log(mean diameter) and log(agitation rate). Microcapsules have a smooth inner membrane (160–220 nm) and a rough, porous outer surface composed of agglomerated UF nanoparticles. Surface morphology is influenced by pH and interfacial surface area. High yields (80–90%) of free-flowing spherical microcapsules with fill content of 83–92 wt% were achieved. The microcapsules are robust and suitable for self-healing applications. During microencapsulation, UF nanoparticles form and deposit on the microcapsule surface, creating a rough surface morphology. This roughness enhances mechanical adhesion when embedded in a polymer and improves self-healing performance. However, maintaining constant pH prevents nanoparticle deposition but reduces yields. Increasing the core-water interfacial area produces microcapsules with smooth surfaces and high yields. Fill content remains high for the required time frame for self-healing polymer production. The microcapsules are composed of a UF shell containing DCPD, with excellent storage and release properties. The process provides a unique toughening mechanism for composite systems. The microcapsules are prepared by in situ polymerization in an oil-in-water emulsion, with the reaction conditions carefully controlled to achieve desired microcapsule properties. The microcapsules are analyzed using optical and electron microscopy to determine size, morphology, and shell thickness. The study highlights the importance of process variables in controlling microcapsule size and surface morphology, which are critical for the performance of self-healing materials.