This study investigates single-layer and double-layer thermally sprayed nickel alloy coatings (bond and top coatings). Ni-5 wt% Al and Ni-20 wt% Cr were used as bond coatings, whereas highly alloyed Ni-based coatings, Hastelloy C276 or Inconel 625 were used as top coatings. Arc spraying (A) and high-velocity oxy-fuel (HVOF) techniques were used to create the coatings on a 304 stainless steel substrate. The samples were studied by performing potentiodynamic polarization tests in a 20 vol% H2SO4 solution at room temperature. The scanning electron microscopy (SEM) with energy dispersive X-ray spectroscopy (EDS) and wavelength dispersive X-ray spectroscopy (WDS) techniques were used to investigate the microstructure and chemical composition of the coatings. The arc sprayed coatings are composed of a lamellar microstructure with low porosities, unmelted particles, and high oxides at the intersplats. A uniform and compact coating with minimal oxides and porosity was achieved for all coatings via HVOF technique. In single-layer coatings, arc spray coating surpasses HVOF coating owing to its oxide layers, which impede sulfuric solution penetration and bolster resistance against electrolyte infiltration. Double-layer coatings, comprising a bonding layer and a top coating, using the same thermal spray method have shown to enhance corrosion resistance.