Mesoscopic Ni particles and nanowires by pulsed electrodeposition into porous Si

We report in this article on the formation of mesoscopic Ni particles and filling of continuous Ni nanowires into porous Si layers of thickness in the range of 0.5–4 μm with anisotropic vertical pores of average diameter in the range of 30–45 nm using pulsed electrodeposition from a Ni salt solution. The effect of pulse duration, number of pulses, and total process time on pore filling was investigated for porous Si with different porosities and porous Si layer thicknesses in the above thickness range. Scanning and transmission electron microscopy were used to characterize the samples. It was found that pore filling starts with Ni nucleation and nanoparticle formation at different points of the pore walls along the whole pore length and continues with nanoparticle coalescence to form continuous Ni nanowires that completely fill the pores. The mechanism involved in pore filling is particle nucleation and diffusion-controlled growth of Ni nanoparticles that coalesce to nanowires. From the beginning of the process, a metal film starts to form on the porous Si surface, and its thickness increases with increasing the process time. However, the presence of this film does not impede further pore filling and nanowire formation into the pores. This supports further the diffusion-controlled growth mechanism. Finally, it was demonstrated that full pore filling and continuous Ni nanowire formation were also achieved under direct current electrodeposition, and the results are quite similar to those obtained with pulsed electrodeposition when the same total deposition time is used in both cases.