As one of the key requirements of the no-flow underfilling process for flip-chip applications, a proper self-fluxing agent must be incorporated in the developed no-flow underfill materials to provide proper fluxing activity during the simultaneous solder reflow and underfill material curing. However, most of fluxing agents have some adverse effects on the no-flow underfill material properties and;assembly reliability. In this paper, we have extensively investigated the effect of the concentration of the selected fluxing agent on the material properties, interconnect integrity and assembly reliability. Through this work, an optimum concentration window of the fluxing agent is obtained and a routine procedure of evaluating fluxing agents is established.