The aim of this work was produce and characterize solid lipid microparticles (SLMs) with different proportions of fully hydrogenated palm oil (FHPO) and palm oil (PO) as wall material (WM) to encapsulate ascorbic acid (AA), using the spray chilling technique. The microparticles were evaluated for surface morphology (SEM), size distribution and mean diameter, polymorphism, encapsulation efficiency, thermal behavior, DSC, and for release profile. The mean particle diameter ranged from 97.80 to 181.29 μm and the micrographs revealed spherical particles and rough surfaces. The encapsulation efficiency ranged from 80.22 to 93.51% and it was influenced by increases in the concentration of PO in each formulation and by the particle size. All the lipid microparticles presented high thermal resistance and had crystalline behavior β′, proving that after atomization the particles preserved the original polymorphic forms of their constituent materials. Moreover, SLMs gradually released ascorbic acid in aqueous medium, following Higuchi kinetic.