The objective of this study is investigation of the effects of process parameters in polyol synthesis of silver nanowires (AgNWs) on the nanostructure morphology and silver nanowire yield for the purpose of process optimization. The AgNWs were synthesized in a batch polyol salt-mediated surfactant-assisted process and characterized by scanning electron microscopy (SEM). The effects of several parameters on morphology and yield, including reagent concentration and molecular weight (MW), temperature, reagent solution preparation, and stirring rate were investigated. Based on this parametric study, the important variables were identified. A design of experiment (DoE) was applied to this set of variables to determine their simultaneous effect on nanowire morphology and yield. An optimum set of parameters was determined and demonstrated to provide very high yield and high length to diameter ratio.