A new synthesis route, based on the hydrolysis of Na 2 [Ni(OH) 4 ] is presented which leads to pure single crystalline nickel hydroxide with crystal sizes up to 0.25 mm. The effect of Natural nickel hydroxide (theophrastite) named after the Greek philosopher Theophratos occurs as a gangue mineral in the magnetite-chromite ores in the Vermion region of northern Greece and in Tasmania (Heazlewood) Australia [1, 2]. Although Williams et al. reported the natural occurrence of nickel hydroxide and demonstrated its authenticity by X-ray powder diffraction, they were unable to ascertain the chemistry [3]. Nickel hydroxide (thermodynamic stable form β-Ni(OH) 2 ) crystallises in the trigonal system with space group P3m1 which is common to several other M(OH) 2 hydroxides ( M ϭ Mg, Mn, Fe, Co, Cd, Ca)[4]. Its structure can be described as a hexagonal close packing of hydroxyl ions (AB-ABA-type) where the cations occupy the octahedral sites. Theophrastite corresponds to the chemical formula Ni(OH) 2 but the natural mineral cannot be investigated in the pure state for it is variably intermixed with diverse hydroxides and possibly an amorphous nickel sulphate. The common way to obtain Ni(OH) 2 synthetically is through precipitation of aqueous NiCl 2 , Ni(NO 3 ) 2 or NiSO 4 solutions with NaOH or KOH solutions in excess [5]. There are also methods using ammonia, sodium carbonate and strong organic bases to synthesise Ni(OH) 2 [6].