Phase evolution during conventional and reactive flash sintering of (Mg,Ni,Co,Cu,Zn)O via in situ X-ray diffraction

Abstract

Reactive flash sintering (RFS) enables the simultaneous synthesis and sintering of ceramics and has been shown to affect the reaction pathway of different materials. Herein, in situ synchrotron X-ray diffraction (XRD) is used to investigate the (Mg,Ni,Co,Cu,Zn)O entropy-stabilized oxide formation during: (i) conventional heating and (ii) RFS under current rate-controlled mode. The same reaction pathway is verified in both instances: the starting rock-salt (RS), spinel (Co3O4), tenorite (CuO), and wurtzite (ZnO) phases transform into a single RS phase with a (1 1 1) to (2 0 0) intensity ratio of 0.67, consistent with a random distribution of the cations into the structure. Pt lattice peak shift from the XRD patterns is used as standard to monitor the sample surface temperature, revealing a strong endothermic reaction during the RS single-phase formation (Pt peaks shift toward higher angles while increasing sample temperature/current density). In RFS, the single-phase RS structure is formed in just 60 s at a furnace temperature of 600°C and a current rate of 220 mA mm−2/min. Therefore, RFS greatly accelerates the synthesis of (Mg,Ni,Co,Cu,Zn)O, however, it does not play a role in the reaction pathway for this material formation.