Ag seed layers were pretreated with 1 : 1,000 diluted nitric acid cleaning solution for 60 s to obtain a clean and oxide-free Ag surface. When an applied potential was less than .800 mV in Ag electroplating, the deposition rate was over 2,000 A/min and the resistivity of Ag deposit was 1.80 μΩ·cm. But the deposit film became rougher with a negative increase in the potential, and it was also observed through measuring the double layer capacitance. The resistivity of Ag film annealed at 350 ℃ for 30 min was decreased from 1.80 μΩ·cm to 1.67 μΩ·cm and the agglomeration of Ag grains was not observed on the surface of the annealed Ag films. To reduce the surface roughness, thiourea was added in the electrolyte and it was decreased below 15 nm.
Dubin V, Lopatin S, Cheung R, in Electrochemical processing in ULSI fabrication I and interconnect and contact metallization: Materials, processes, and reliability, Andricacos PC, Dukovic JO, Mathad GS, Oleszek GM, Rathore HS, Simpson CR, PV 98-6, p. 12, The Electrochemical Proceedings Series, Pennington, NJ (1999)