Microwave is advantageous for nanoparticle synthesis because nanostructured crystals and mono-dispersed nanoparticle size can be obtained due to the rapid growth induced by quick thermal response. In previous studies, it has been confirmed that an individual application of two-stage irradiation and anti-solvent addition is effective in promoting stable nucleation and smaller particle generation. Nevertheless, to date no studies have been reported in applying the two methods above simultaneously and examining their synergistic effect. This study, therefore, aims to investigate the possibility of producing finer particles using a stable operation without any superheating and abrupt bubble growth. From the experimental data, it is evident that the beneficial combined effect of two-stage irradiation and addition of anti-solvent on the stable finer nanoparticle formation could be observed and confirmed. It is expected that the findings and recommendations from this work may be useful in optimizing two-stage microwave-assisted nanoparticle synthesis with an addition of anti-solvent.