Various studies were performed to fabricate self-assembling nanoobjects out of noble metals, but a few efforts were made for engineering iron-based nanorods toward sell-assembling blocks. In this regard β-FeOOH nanorods were fabricated in various sizes to achieve iron-based rod nanoblocks with self-assembling potential. Hydrolysis of ferric ions in various concentrations was successfully developed as a novel approach to control the growth of β-FeOOH crystals and tuning the length of rods in the nano range, below 100 nm. It was found that the concentration of ferric ion has no effect on the widths of nanorods, but the length was affected. By increasing the concentration of ferric ions, an increase in the length of nanorods and an increase of aspect ratio occurred. All sizes of the resulting FeOOH nanorods exhibited mesoporous feature, but interestingly the hysteresis loops were different due to different pore patterns. In fact, pores on the larger particles were more uniform in size and shape. Nanorods of small length did not make suitable interactions toward ordered phase formation, but rods with the mean length of about 90 nm or longer, at a certain concentration, were able to form nematic phases. The large (∼+40 mV) zeta-potential of nanorods prevents formation of dense arrays, and just bundle-like structures were observed. These findings highlight the importance of size, surface charge, and concentration of nanoobjects in the formation of 3D structures. The developed technique in the fabrication of β-FeOOH nanorods provides pure structures that are free from any size-controlling agent. These pure structures are suitable for further functionalization or coating. Self-assembling nanoobjects is a developing field in nanotechnology, and therefore studies can help our understanding over the assembling process.