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Abstract: We have regulated the permeability in macroporous alumina materials by manipulating the connectivity of the pore phase and the sizes of the smallest constrictions between connected pores. Templating with particle-coated expandable polymeric spheres (EPS) significantly increased the fraction of isolated pore clusters, and reduced both the sizes and the number of connections with neighboring pores, as determined by three-dimensional evaluation with X-ray micro-computed tomography. The stable particle coating, applied onto the EPS surfaces using polyelectrolyte multilayers, reduced the volume expansion and the coalescence of the EPS at elevated temperatures, which reduced the simulated permeability by as much as two orders of magnitude compared to templating with uncoated EPS in materials of similar porosities. We show that the Katz–Thompson model accurately predicts the permeability for the macroporous alumina materials with porosities of 46–76%. This suggests that the permeability to fluid flow in these materials is governed by the smallest constrictions between connected pores: the critical pore throat diameter. [Copyright &y& Elsevier]