We performed stacking experiments on Si dies using annular tungsten TSVs (Through Silicon Vias) and Cu studs with low-volume solder micro-bumps. Unlike standard 100- micron C4 (Controlled Collapse Chip Connection) solder balls, very small solder volumes (< 6 microns in height) form IMC (InterMetallic Compounds) in the junctions during the bonding or reflow processes. The two interconnect metallurgies of Cu/Ni/In and Cu/Sn joints were considered for low-volume lead-free solder micro-bumps for 3D integration. A previous study on these metallurgies  showed that the Cu/Sn joints form thermally stable intermetallics while in the Cu/Ni/In joints, some indium solder remains unreacted due to the presence of the Ni barriers. The shear testing on the stacked systems showed that the die stacks with Cu/Sn joints exhibit higher shear strengths than those with Cu/Ni/In joints. However the impact shock testing on the systems revealed that the die stacks with Cu/Sn joints are less resistant to mechanical shocks than the systems with Cu/Ni/In joints. This new work focuses on thermal cycle testing of the die stack systems with the Cu/Ni/In and Cu/Sn interconnections. Preliminary thermal cycle testing on the die stack systems with Cu/Ni/In joints showed that the joints are stable against thermal cycle stresses for thousands of cycles. To quickly compare the systems with two metallurgies, we mounted the Si die stacks onto organic substrates to impose additional stresses on the systems. In addition to standard DTC (Deep Thermal Cycle) tests, we also conducted a HAATS (Highly accelerated Air to Air Thermal Shock) test  with a short cycle time to reduce the testing time. The DTC and HAATS tests showed that the stacked systems with Cu/Ni/In joints had fewer failures and smaller increases in the electrical resistances of the joints during the tests than the systems with Cu/Sn joints. © 2010 IEEE.