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Lead-free solder reflow process has presented challenges to no-flow underfill material and assembly. The currently available no-flow underfill materials are mainly designed for eutectic Sn-Pb solders. This paper presents the assembly of lead-free bumped flip-chip with developed no-flow underfill materials. Epoxy resin/HMPA/metal AcAc/Flux G system is developed as no-flow underfills for Sn/Ag/Cu alloy bumped flip-chips. The solder wetting test is conducted to demonstrate the fluxing capability of the underfills for lead-free solders. A 100% solder joint yield has been achieved using Sn/Ag/Cu bumped flip-chips in a no-flow process. A scanning acoustic microscope is used to observe the underfill voiding. The out-gassing of HMPA at high curing temperatures causes severe voiding inside the package. A differential scanning calorimeter (DSC) used to study the curing degree of the underfill after reflow with or without post-cure. The post-curing profiles indicate that the out-gassing of HMPA would destroy the stoichiometric balance between the epoxy and hardener, and result in a need for high temperature post-cure. The material properties of the underfills are characterized and the influence of underfill out-gassing on the assembly and material properties is investigated. The impact of lead-free reflow on the material design and process conditions of no-flow underfill is discussed.