Field-emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM) were employed to characterize the surface morphology of the synthesized samples. The energy-dispersive X-ray spectroscopy (EDS) shows that all the deposited metals remain on the catalyst. This can be seen in the EDS spectra in Figure which shows distinct elemental peaks corresponding to Ni, Co, Fe, Mo, S, and O in NiFeCo-LDH, NiFeCo-Mo(doped)-LDH, MoS 2 @NiFeCo-LDH, and MoS 2 @NiFeCo-Mo(doped)-LDH. Moreover, the SEM-EDS elemental mapping of MoS 2 @NiFeCo-Mo(doped)-LDH validates the uniform distribution of the elements within the catalyst (Figure ). The SEM-EDS maps for other heterostructures are presented in Figure and affirm the uniform element distribution within the LDHs.