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Abstract High‐power piezoelectric applications are predicted to share approximately one‐third of the lead‐free piezoelectric ceramic market in 2024 with alkaline niobates as the primary competitor. To suppress self‐heating in high‐power devices due to mechanical loss when driven by large electric fields, piezoelectric hardening to restrict domain wall motion is required. In the present work, highly effective piezoelectric hardening via coherent plate‐like precipitates in a model system of the (Li,Na)NbO₃(LNN) solid solution delivers a reduction in losses, quantified as an electromechanical quality factor, by a factor of ten. Various thermal aging schemes are demonstrated to control the average size, number density, and location of the precipitates. The established properties are correlated with a detailed determination of short‐ and long‐range atomic structure by X‐ray diffraction and pair distribution function analysis, respectively, as well as microstructure determined by transmission electron microscopy. The impact of microstructure with precipitates on both small‐ and large‐field properties is also established. These results pave the way to implement precipitate hardening in piezoelectric materials, analogous to precipitate hardening in metals, broadening their use cases in applications. 

In this work with a model system (Ba,Ca)TiO3, we analyze the morphologies of CaTiO3-rich precipitates and their impacts on the microstructures in their surrounding BaTiO¬3-rich matrix. Also, the response of ferroelectric domains around CaTiO3-rich precipitates during heating and cooling is observed in-situ with transmission electron microscopy. Domains attached to precipitates are observed remaining unchanged up to the Curie point at which they disappear. During cooling, domains are observed to form in the vicinity of precipitates and being held in place down to room temperature. Both observations corroborate previous findings that precipitates act as domain pinning points, behaving in a similar manner to earlier experiments with electrical field biasing. Dislocations are often seen around precipitates in the matrix grain and are observed interfering with domains during heating cycles. Dislocations may provide an additional mechanism to restrict domain wall motion and offer a greater piezoelectric hardening effect. 

Precipitates have recently been found to significantly enhance the mechanical quality factor in piezoelectric ceramics. Such a piezoelectric hardening effect was attributed to strong interactions between ferroelectric domains and precipitates. In the present work, the response of domains to applied electric fields is observed in situ via transmission electron microscopy in aged (Ba, Ca)TiO3 ceramics with precipitates to reveal the underlying mechanism of this phenomenon. Ferroelectric domains in the Ba-rich matrix grain are observed to be more concentrated near non-polar Ca-rich precipitates. With increasing applied voltage, domains separate from precipitates merge together first, while those near precipitates persist to higher voltages. During ramping down, domains nucleate from precipitates. These direct observations confirm the strong interactions between ferroelectric domains and precipitates in piezoelectric ceramics.