This paper describes the wet-chemistry synthesis of highly crystalline hexagonal flakes of Ni-Fe layered double hydroxide (LDH) produced at temperature as low as 100 °C. The flakes with diameter in the range of 0.5–1.5 μm and the thickness between 15 and 20 nm were obtained by homogeneous precipitation method with the use of triethanolamine (TEA) and urea. By analyzing the intermediate products, it is suggested that, differently from previous reports, a thermodynamically metastable iron oxyhydroxide and Ni-TEA complex are firstly formed at room temperature. Subsequently, when the mixture is heated to 100 °C and the pH increases due to the thermal decomposition of urea, Ni2+ and Fe3+ are slowly released and then recombine, thus leading to formation of pure, highly-crystalline Ni-Fe LDH flakes. This material showed promising results as an electrocatalyst in oxygen evolution reaction (OER) providing an overpotential value of 0.36 V.

Nickel-iron layered double hydroxides are known to be one of the most highly active catalysts for the oxygen evolution reaction in alkaline conditions. The high electrocatalytic activity of the material...

Nickel–iron-layered double hydroxide (NiFe LDH) platelets with high morphological regularity and submicrometre lateral dimensions were synthesized using a homogeneous precipitation technique for highly efficient catalysis of the oxygen evolution reaction (OER). Considering edge sites are the point of activity, efforts were made to control platelet size within the synthesized dispersions. The goal is to controllably isolate and characterize size-reduced NiFe LDH particles. Synthetic approaches for size control of NiFe LDH platelets have not been transferable based on published work with other LDH materials and for that reason, we instead use postsynthetic treatment techniques to improve edge-site density. In the end, size-reduced NiFe LDH/single-wall carbon nanotube (SWCNT) composites allowed to further reduce the OER overpotential to 237 ± 7 mV (<L> = 0.16 ± 0.01 μm, 20 wt% SWCNT), which is one of the best values reported to date. This approach as well improved the long-term activity of the catalyst in operating conditions.