A complex approach to assessing porous structure of structured ceramics obtained by SPS technique

Spark plasma sintering (SPS) is a highly prospective technology providing rapid consolidation of nano-disperse compositions into structured ceramics with complex structural organization. Characterizing pore structure of such systems remains a challenge due to different types, size and shape of the pores as well as structural defects occurring in the material, thus requiring special methods to quantify certain porosity type. The paper presents a complex approach to studying structure of SPS hematite-based structured ceramics. The method involves a number of gas, intrusion and electron microscopy probing techniques to characterize open and closed pores in the ceramics bulk. Low temperature nitrogen sorption has been implemented to estimate open micro- and mesoporosity in the size range 0.7–50 nm using BET, BJH and t-plot methods to process experimental data. Additionally, structural peculiarities of consolidated structured ceramics have been studied using temperature-programmed reduction (TPR) with the kinetic analysis of the results being carried out. Volume of macropores sized above 50 nm has been measured with mercury intrusion. Closed pores and structural defects have been quantified with SEM and FIB/SEM tomography. By comparing experimental and estimated results we have shown that addressing all porosity types provides a highly precise structural characterization of the material. [Display omitted] •A complex approach to microstructural analysis of nanostructured SPS ceramics was presented.•A bunch of gas, intrusion and microscopic methods were applied for open/closed porosity determination in nanoceramics.•Kinetic TPR analysis for structural changes in nanoceramic was carried out.•3D pore visualization for nanoceramics was provided via SEM/FIB tomography•Porosity calculations were performed via BET, BJH, t-plot, Washburn equation, FEI Avizo 9.1 software results.