10 March 2025 3 928 Report

I’m trying to identify the reduction peak of Ni²⁺ ions on either a nickel or copper working electrode using a three-electrode setup (Pt wire as the counter electrode and Ag/AgCl as the reference). I’ve tested two different solution compositions:

  • High-Concentration Nickel BathNiSO₄·6H₂O: 250 g/L (providing Ni²⁺) NiCl₂·6H₂O: 50 g/L (to enhance conductivity) H₃BO₃: 30 g/L (buffering the pH) pH = 4.0–5.5 Temperature: 50–60 °C
  • Dilute Nickel Solution5 mM NiCl₂·6H₂O 0.2 M Boric Acid (B(OH)₃)
  • My linear sweep voltammetry (LSV) parameters are:

    • Potential range: 0 V to –2 V (vs. Ag/AgCl)
    • Scan rate: 50 mV/s

    In both cases, the resulting LSV shows a nearly constant current of about 2.5 × 10⁻⁵ A from 0 to –0.7 V, followed by a sudden drop to around –2.5 × 10⁻⁵ A from –0.7 V down to –2 V. This creates a “Z-shaped” curve instead of producing a distinct reduction peak for Ni²⁺.

    I would like to understand why this abrupt change in current (the “Z shape”) occurs and why I’m not observing a clear nickel reduction peak. Any insights or suggestions on improving the setup or parameters to obtain a well-defined nickel reduction peak would be greatly appreciated.

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