A study on the effect of synthesis parameters on the size of nickel particles in sol–gel derived Ni–SiO2–Al2O3 nanocomposites

Abstract

The present work deals with the synthesis of Ni–SiO2–Al2O3 nanocomposites fabricated by embedding nickel oxide particles, obtained from hexahydrated nickel nitrate [Ni(NO3)2 · 6H2O], in matrixes with different molar percents of Silica/Alumina, through sol–gel method based on hydrolysis and condensation of tetraethylorthosilicate (TEOS) and Aluminum Isopropoxide [Al(OC3H7)3] alkoxides. Due to the various factors, e.g., pH, EtOH/TEOS/H2O ratio, Si/Ni ratio etc., influencing the nickel grain size of the nanocomposites, Taguchi robust design method of system optimization was used to determine the percent of contribution (%ρ) of each factor. The nanocomposites were reduced in a flow of hydrogen and nitrogen gas at 700 °C for half an hour. The nickel grain size in the nanocomposites was determined by utilizing Scherrer`s method and XRD patterns. The smallest nickel grain size obtained from the Taguchi orthogonal array was about 24 nm, later confirmed by TEM observations. After optimization of the controlling factors, a nickel grain size of 15.4 nm was obtained. It was found that the SiO2/Al2O3 molar ratio of the matrix had the most influence on the nickel grain size (29.22%) and the Water/TEOS molar ratio stood in second place (21.44%). It was illustrated that the starting temperature of the aluminum isopropoxide had the least influence on the nickel grain size.