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Despite significant interest in their functional properties, the mechanical behavior of high-entropy oxides (HEOs) is not well studied, particularly at elevated temperatures. Bulk (Co,Cu,Mg,Ni,Zn)O (transition metal (TM)-HEO) samples were deformed under compression at applied stresses and temperatures ranging from 5 to 31 MPa and 600 to 850 °C, respectively. All of the deformation conditions result in creep stress exponents of n < 3, indicating that TM-HEO exhibits superplastic deformation. A transition from structural to solution-precipitation-based superplasticity is observed during deformation above 650 °C. Additionally, TM-HEO exhibits shear-thickening behavior when deformed at stresses above 9 MPa. The formation and behavior of a Cu-rich tenorite secondary phase during deformation is identified as a key factor underpinning the deformation mechanisms. The microstructure and phase state of TM-HEO before deformation also influenced the behavior, with finer grain sizes and increasing concentrations of Cu-rich tenorite, resulting in the increased prevalence of solution-precipitation deformation. While complex, the results of this study indicate that TM-HEO deforms through known superplastic deformation mechanisms. Superplasticity is a highly efficient manufacturing method and could prove to be a valuable strategy for forming HEO ceramics into complex geometries. 

Magnesium (Mg) alloys are promising lightweight structural materials whose limited strength and room‐temperature ductility limit applications. Precise control of deformation‐induced twinning through microstructural alloy design is being investigated to overcome these deficiencies. Motivated by the need to understand and control twin formation during deformation in Mg alloys, a series of magnesium‐yttrium (Mg–Y) alloys are investigated using electron backscatter diffraction (EBSD). Analysis of EBSD maps produces a large dataset of microstructural information for >40000 grains. To quantitatively determine how processing parameters and microstructural features are correlated with twin formation, interpretable machine learning (ML) is employed to statistically analyze the individual effects of microstructural features on twinning. An ML classifier is trained to predict the likelihood of twin formation, given inputs including grain microstructural information and synthesis and deformation conditions. Then, feature selection is used to score the relative importance of these inputs for twinning in Mg–Y alloys. It is determined that using information only about grain size, grain orientation, and total applied strain, the ML model can predict the presence of twinning and that other parameters do not significantly contribute to increasing the model's predictive accuracy. Herein, the utility of ML for gaining new fundamental insights into materials processing is illustrated. 

High‐entropy oxides (HEOs) are being extensively studied for various functional applications, but there is limited research into the mechanical behavior of these materials, especially at elevated temperatures. Bulk (Co, Cu, Mg, Ni, Zn)O (transition metal (TM)‐HEO) samples are formed into dome shapes at 800 °C and 70 kPa. Deformation experiments and finite element analysis (FEA) reveal that TM‐HEO has a creep stress exponent ofn = 0.6, indicating that TM‐HEO deforms through superplastic deformation and exhibits shear‐thickening behavior. Comparisons of experimental strain rates to those calculated using existing superplasticity mechanism models signify that TM‐HEO deforms through grain boundary sliding accommodated by a solution‐precipitation mechanism from a secondary phase. A Cu‐rich tenorite phase, commonly observed in the grain boundaries of TM‐HEO, is proposed as the secondary phase facilitating deformation. It is important to highlight here that the superplastic deformation behavior in TM‐HEO is active under modest temperature and pressure conditions, as noted above. Low‐temperature superplastic deformation will provide a powerful method of manufacturing HEO ceramics into net shape parts, greatly expanding their potential applications. 

Bulk, polycrystalline (Co, Cu, Mg, Ni, Zn)O was synthesized using solid-state sintering. Micropillars were prepared and mechanically deformed along three crystallographic orientations: (001), (101), and (111). Pillars (001) and (111) cracked, while Pillar (101) remained intact. Pillars (001) and (101) exhibited activated slip systems, confirmed by a large stress drop, and the presence of slip bands, respectively. Schmid factor (SF) analysis was performed to examine the effect of grain orientations on dislocation activity and slip behavior. SF values range from 0 to 0.5, with non-zero values indicating potential for slip. Six slip systems exist in the (Co, Cu, Mg, Ni, Zn)O rock salt crystal structure: 1/2⟨110⟩11¯0. For the (001) orientation, four slip systems are potentially active (SF = 0.5). For the (101) orientation, there are four potentially active slip systems (SF = 0.25). For the (111) orientation, no potentially active slips systems exist (SF = 0). Dislocation structures, which were observed post-compression via transmission electron microscopy, demonstrated variations in size, number, and distribution across the pillar, depending on micropillar orientation. Entangled dislocations created misorientation in Pillar (001), which led to the possible formation of subgrains, while singular dislocations were observed in Pillar (101), and a lack of dislocations was observed in Pillar (111). Zener–Stroh type dislocation entanglement-mediated cracking is the proposed cause of the transgranular-type cracks in Pillar (001). The possible subgrain formation, or lack of formation, respectively, caused intergranular-type cracks to additionally form in Pillar (001), while Pillar (111) only exhibited transgranular-type brittle fracture. In combination, these findings highlight the importance of dislocation activity, without the need for elevated temperature, and grain orientation in controlling the mechanical deformation response in single-phase (Co, Cu, Mg, Ni, Zn)O. 

Abstract Entropy‐stabilized oxide (ESO) research has primarily focused on discovering unprecedented structures, chemistries, and properties in the single‐phase state. However, few studies discuss the impacts of entropy stabilization and secondary phases on functionality and in particular, electrical conductivity. To address this gap, electrical transport mechanisms in the canonical ESO rocksalt (Co,Cu,Mg,Ni,Zn)O are assessed as a function of secondary phase content. When single‐phase, the oxide conducts electrons via Cu⁺/Cu²⁺small polarons. After 2 h of heat treatment, Cu‐rich tenorite secondary phases form at some grain boundaries (GBs), enhancing grain interior electronic conductivity by tuning defect chemistry toward higher Cu⁺carrier concentrations. 24 h of heat treatment yields Cu‐rich tenorite at all GBs, followed by the formation of anisotropic Cu‐rich tenorite and equiaxed Co‐rich spinel secondary phases in grains, further enhancing grain interior electronic conductivity but slowing electronic transport across the tenorite‐rich GBs. Across all samples, the total electrical conductivity increases (and decreases reversibly) by four orders of magnitude with heat‐treatment‐induced phase transformation by tuning the grains’ defect chemistry toward higher carrier concentration and lower migration activation energy. This work demonstrates the potential to selectively grow secondary phases in ESO grains and at GBs, thereby tuning the electrical properties using microstructure design, nanoscale engineering, and heat treatment, paving the way to develop many novel materials.