Abstract: (388 Views)
Producing high-purity iron powders with controlled particle morphology is essential for advanced powder metallurgy, additive manufacturing, and functional materials. However, achieving precise morphological control in environmentally benign, additive-free electrolytes remains challenging. This study systematically investigates the galvanostatic electrodeposition of iron powder from sulfate-based electrolytes containing 10.0 and 50.0 g·L⁻¹ Fe²⁺, focusing on the interplay between current density, pH evolution, deposition efficiency, and particle structure. A clear transition from compact, adherent deposits at low current densities to dendritic, easily detachable powders at higher values was observed. SEM analysis revealed well-defined dendritic aggregates at 7 A·dm⁻² (30–80 μm), whereas highly fragmented, porous agglomerates formed at 10 A·dm⁻², accompanied by fine-scale fragmentation driven by intense hydrogen evolution. XRD confirmed pure α-Fe for current densities up to 7 A·dm⁻², while partial oxidation to Fe₃O₄ occurred at 10 A·dm⁻²; EDX mapping further supported this surface oxidation. The deposited mass increased linearly with current density for both Fe²⁺ concentrations, with regression models yielding R² values above 0.96. Current efficiency decreased at high current densities due to enhanced parasitic reactions. Overall, the results demonstrate that galvanostatic electrodeposition in additive-free sulfate media enables controlled synthesis of iron powders, with tunable morphology and phase purity governed primarily by current density and electrolyte composition.
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- Galvanostatic iron powder deposition was investigated using additive-free sulfate electrolytes at two Fe²⁺ concentrations.
- SEM, XRD, and EDX analyses revealed a strong current-density-driven transition from dendritic α-Fe to fragmented Fe/Fe₃O₄ morphologies.
- Powder yield increased linearly with current density, with empirical models showing excellent agreement with experiments (R² > 0.96).
- High current densities induced intense hydrogen evolution, reduced current efficiency, and promoted multiscale fragmentation of the deposits.
- The environmentally benign electrolyte system provides a robust platform for controlled, high-purity iron powder production relevant to advanced materials processing.