Liquid-Phase Synthesis and Regulatory Mechanisms of Nano-Nickel Powders for MLCC Inner Electrodes

Driven by the demand for miniaturization, high capacitance, and enhanced reliability in high-performance multilayer ceramic capacitors (MLCCs), the continuous thinning of inner electrode layers imposes increasingly stringent requirements on the size, distribution, morphology, and dispersion of nano-nickel powders. We systematically investigate how functional additives regulate the nucleation, growth, and microstructural evolution of nano-nickel synthesized via hydrazine-driven liquid-phase reduction of nickel sulfate. The results demonstrate that the alkanolamine complexing agent (TAC) significantly refines the average particle size and morphology of the nano-nickel through coordination effects. Furthermore, inorganic sulfur salts (ISP), acting via surface adsorption to passivate growth sites and provide catalytic effects, enable a precise and continuous reduction in the average particle diameter from 330 nm down to 60 nm at a mere trace dosage of ~10−7 mol/L. Regarding dispersion optimization, highly dispersed face-centered cubic (FCC) nano-nickel was successfully prepared by introducing multidentate carboxylate (NNA). High-resolution transmission electron microscopy (HRTEM) was employed to unveil, for the first time, the crystallographic origin of the anomalous surface protrusions typically observed in conventional reaction systems. We confirmed that the family of 101¯0 crystal planes within these regions, which exhibits interfacial angles of 58.7° and 58.3°, corresponds to a thermodynamically metastable hexagonal close-packed (HCP) nickel phase originating from atomic stacking faults induced by rapid growth kinetics. To address this microstructural defect, a thioether-based amino acid (TAA) was introduced. TAA effectively suppresses the anisotropic growth of the metastable HCP phase through the strong steric hindrance of its long side chains and its selective adsorption onto high-energy facets.