Objectives The objectives of this study were to assess demineralized dentin porosity and quantify the different porous features distribution within the material using mercury intrusion porosimetry (MIP) technique. We compared hexamethyldisilazane (HMDS) drying and lyophilization (LYO) (freeze-drying) in sample preparation. Methods Fifty-six dentin discs were assigned into three groups. The control (CTR) group discs were superficially acid-etched (15 s 37% H3PO4) to remove the smear layer and then freeze-dried whereas LYO and HMDS groups samples were first totally demineralized using EDTA 0.5 M and then freeze-dried and HMDS-dried respectively. MIP was used to determine open porosity and pore size distribution of each pair of samples. Field emission scanning electron microscopy (FESEM) was used to illustrate the results. Results The results showed two types of pores corresponding either to tubules and micro-branches or to inter-fibrillar spaces created by demineralization. Global porosity varied from 59% (HMDS-dried samples) to 70% (freeze-dried samples). Lyophilization drying technique seems to lead to less shrinkage than HMDS drying. FESEM revealed that collagen fibers of demineralized lyophilized samples are less melted together than in the HMDS-dried samples. Significance Demineralized dentin porosity is a key parameter in dentin bonding that will influence the hybrid layer quality. Its characterization could be helpful to improve the monomers infiltration.