The present study deals with the application of sequential procedure (i.e. steepest ascent) to obtain the optimum values of process parameters for conducting friction stir welding (FSW) experiments. A vertical milling machine is modified by fabricating fixture and tool ( H13 material) for performing FSW operation to join AA7039 plates. The steepest ascent technique is employed to design the experiments at different rotational speed, welding speed, and tilt angle. The ultimate tensile strength is considered as a performance characteristic for deciding the optimal levels. The mechanical and metallurgical characteristics of the joints are studied by executing tensile and microhardness tests. It is concluded from the graphical analysis of the steepest ascent technique that the optimal maximum and minimum values are 1812–1325 r/min for rotational speed, 43–26 mm/min for welding speed, and 2°–1.3° for tilt angle, respectively. Besides, optical microscope and scanning electron microscope are utilized for microstructural and fractographic analyses for a better understanding of the process.