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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. 

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. 

Abstract The rocksalt structured (Co,Cu,Mg,Ni,Zn)O entropy-stabilized oxide (ESO) exhibits a reversible phase transformation that leads to the formation of Cu-rich tenorite and Co-rich spinel secondary phases. Using atom probe tomography, kinetic analysis, and thermodynamic modeling, we uncover the nucleation and growth mechanisms governing the formation of these two secondary phases. We find that these phases do not nucleate directly, but rather they first form Cu-rich and Co-rich precursor phases, which nucleate in regions rich in Cu and cation vacancies, respectively. These precursor phases then grow through cation diffusion and exhibit a rocksalt-like crystal structure. The Cu-rich precursor phase subsequently transforms into the Cu-rich tenorite phase through a structural distortion-based transformation, while the Co-rich precursor phase transforms into the Co-rich spinel phase through a defect-mediated transformation. Further growth of the secondary phases is controlled by cation diffusion within the primary rocksalt phase, whose diffusion behavior resembles other common rocksalt oxides. Graphical abstract 

Abstract High-entropy oxides (HEO) with entropic stabilization and compositional flexibility have great potential application in batteries and catalysis. In this work, HEO thin films were synthesized by pulsed laser deposition (PLD) from a rock-salt (Co 0.2 Ni 0.2 Cu 0.2 Mg 0.2 Zn 0.2 )O ceramic target. The films exhibited the target’s crystal structure, were chemically homogeneous, and possessed a three-dimensional (3D) island morphology with connected randomly shaped nanopores. The effects of varying PLD laser fluence on crystal structure and morphology were explored systematically. Increasing fluence facilitates film crystallization at low substrate temperature (300 °C) and increases film thickness (60–140 nm). The lateral size of columnar grains, islands (19 nm to 35 nm in average size), and nanopores (9.3 nm to 20 nm in average size) increased with increasing fluence (3.4 to 7.0 J/cm 2 ), explained by increased kinetic energy of adatoms and competition between deposition and diffusion. Additionally, increasing fluence reduces the number of undesirable droplets observed on the film surface. The nanoporous HEO films can potentially serve as electrochemical reaction interfaces with tunable surface area and excellent phase stability. Graphical abstract