Reliability assessment of ultra-thin HfO2 films deposited on silicon wafer

Highlights: ► Nano-mechanical properties on annealed ultra-thin HfO2 film are studied. ► By AFM analysis, hardness of the crystallized HfO2 film significantly increases. ► By nano-indention, the film hardness increases with less contact stiffness. ► Quality assessment on the annealed ultra-thin films can thus be achieved. - Abstract: Ultra-thin hafnium dioxide (HfO2) is used to replace silicon dioxide to meet the required transistor feature size in advanced semiconductor industry. The process integration compatibility and long-term reliability for the transistors depend on the mechanical performance of ultra-thin HfO2 films. The criteria of reliability including wear resistance, thermal fatigue, and stress-driven failure rely on film adhesion significantly. The adhesion and variations in mechanical properties induced by thermal annealing of the ultra-thin HfO2 films deposited on silicon wafers (HfO2/SiO2/Si) are not fully understood. In this work, the mechanical properties of an atomic layer deposited HfO2 (nominal thickness ≈10 nm) on a silicon wafer were characterized by the diamond-coated tip of an atomic force microscope and compared with those of annealed samples. The results indicate that the annealing process leads to the formation of crystallized HfO2 phases for the atomic layer deposited HfO2. The HfSixOy complex formed at the interface between HfO2 and SiO2/Si, where the thermal diffusion of Hf, Si, and O atoms occurred. The annealing process increases the surface hardness of crystallized HfO2 film and therefore the resistance to nano-scratches. In addition, the annealing process significantly decreases the harmonic contact stiffness (or thereafter eliminate the stress at the interface) and increases the nano-hardness, as measured by vertically sensitive nano-indentation. Quality assessments on as-deposited and annealed HfO2 films can be thereafter used to estimate the mechanical properties and adhesion of ultra-thin HfO2 films on SiO2/Si substrates.