A parallel solution combustion synthesis technique was developed for combinatorial materials studies. The vigorous combustion reactions were successfully limited in the microreactors by using a substrate-net-mask microreactor system and the lowest adoptable furnace temperature. Using this technique, a luminescent materials library of Y3Al5O12/Tb(chi) was synthesized with the aid of an ink-jet delivery system. Structure and luminescence characterizations were implemented using X-ray diffraction and UV/X-ray spectroscopies, respectively. The results show that this technique is reliable and applicable to combinatorial study of powder materials with high synthesis temperature.