Yttrium aluminum garnet powders by nitrate decomposition and nitrate–urea solution combustion reactions—a comparative study

Abstract

Precursors for yttrium aluminum garnet (Y 3Al 5O 12—YAG) were synthesized by simple decomposition of concentrated aqueous solution of nitrates and combustion of concentrated aqueous solution of nitrates with urea on a heater. The precursor formed by the former reaction was granules of agglomerated powder while that from the latter reaction was a voluminous and porous sponge-like mass. Both precursors were ground to powders and subjected to detailed thermogravimetric–differential thermal analysis and X-ray diffraction studies. The precursor from the simple decomposition of nitrates exhibited a total loss in weight of about 18% in stages (25 to 300 °C and 300 to 600 °C) accompanied by endotherms—characterized as processes of dehydration of absorbed moisture and decomposition of residual nitrates, respectively. The as formed precursor and that heated to 820 °C were amorphous. Crystallization to YAG phase occurred from an amorphous oxide characterized by an exotherm above 820 °C with no loss of weight. The precursor from nitrate–urea combustion reaction was found to exhibit a weight loss of 2.5% accompanied by a shallow endotherm in the range of 25 to 300 °C—characterized as the process of dehydration of absorbed moisture. No further weight loss or heat effect was noticed, confirming it to be chemically pure YAG. This as formed precursor was found to be crystalline YAG. The difference in chemical composition of the precursors formed by these two reactions is attributed to the difference in the actual reaction temperatures during their formation—lower reaction temperature for the endothermic decomposition of nitrates and higher reaction temperature for the exothermic combustion associated with the formation of a bright flame. The morphology of the precursor powder formed by the former reaction exhibited only cracks while that of the precursor from the latter reaction exhibited pores and voids. The precursor from the former reaction was calcined at 1100 °C to form into chemically pure YAG. Zeta potential variation with pH for the aqueous suspensions of the crystalline YAG powders from both the reactions exhibited a maximum value in the range of 40 to 50 mV around a pH of 4, indicating stability of these dispersions towards coagulation at this pH. Particle size distribution of wet ground powders (slurries with 20%, v/v, solid at a pH of 4) showed that the powder from combustion reaction could be formed into a finer size than that from simple nitrate decomposition, indicating the agglomerates of combustion reaction were softer.