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The parallel evolution of microstructure development via grain size changes from a nano-to-micron size regime toward multiferroic property development has been established in this research work. This kind of observation is not present in the literature in this research area, and studies of the link between morphological properties and ferroelectric properties of multiferroic materials have been focusing solely on the product of the ultimate sintering temperature, mostly neglecting the parallel evolutions of morphological properties and their relationship at varied chosen sintering temperatures. Holmium manganese oxide and yttrium manganese oxide were both prepared via high-energy ball milling (HEBM) in a hardened steel vial for 12 h. The pressed pellet went through multi-sample sintering, whereas the samples were sintered starting from 600 to 1250°C with 50°C increments for any one sample being subjected to only one sintering temperature. Orthorhombic HoMn2O5 and YMn2O5 phases were observed to exist in both as milled powder. The degree of crystallinity increased with increasing sintering temperature. Hexagonal HoMnO3 peaks were observed for sintering temperature ≥1050°C. As for YMnO3 series, the single phase of hexagonal YMnO3 started to appear at sintering temperature ≥1000°C. FESEM micrographs revealed that as the sintering temperature increased, the grain size increased, consequently increasing the geometric ferroelectric behavior. The polarization-electric field (P-E) plot reveals that HoMnO3 and YMnO3 are highly leaky ferroelectrics with a P-E curve shape different from the normal shape of highly insulating ferroelectrics. It shows that the remanent polarization and electric field increased generally with increasing grain size. For both series, there existed a difference based on their difference of crystallinity, microstructure data, and phase purity changes. Larger grain size is known to give ease for polarization to take place.

Evolution of Nanometer-to-Micrometer Grain Size in Multiferroic Properties of Polycrystalline Holmium and Yttrium Manganite