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This paper describes the wet-chemistry synthesis of highly crystallinehexagonal flakes of Ni-Fe layered double hydroxide (LDH) produced attemperature as low as 100 oC. The flakes with diameter in the range of 0.5-1.5um and the thickness between 15 and 20 nm were obtained by homogeneousprecipitation method with the use of triethanolamine (TEA) and urea. Byanalyzing the intermediate products, it is suggested that, differently fromprevious reports, a thermodynamically metastable iron oxyhydroxide and Ni-TEAcomplex are firstly formed at room temperature. Subsequently, when the mixtureis heated to 100 oC and the pH increases due to the thermal decomposition ofurea, Ni2+ and Fe3+ are slowly released and then recombine, thus leading toformation of pure, highly-crystalline Ni-Fe LDH flakes. This material showedpromising results as an electrocatalyst in oxygen evolution reaction (OER)providing an overpotential value of 0.36 V.

Low-temperature synthesis of high quality Ni-Fe layered double hydroxides hexagonal platelets