For heterogeneous integration in many More-than-Moore applications, surface preparation is the key step to realizing well-bonded multiple substrates for electronics, photonics, fluidics and/or mechanical components without a degradation in performance. Therefore, it is critical to understand how various processing and environmental conditions affect their surface properties. In this paper, we investigate the effects of oxygen plasma and humidity on some key surface properties such as the water contact angle, roughness and hardness of three materials: silicon (Si), silicon dioxide (SiO 2) and glass, and their impact on bondability. The low surface roughness, high surface reactivity and high hydrophilicity of Si, SiO 2 and glass at lower activation times can result in better bondability. Although, the surface reactivity of plasma-ambient-humidity-treated Si and SiO 2 is considerably reduced, their reduction of roughness and increase of hydrophilicity may enable good bonding at low temperature heating due to augmented hydroxyl groups. The decrease of hardness of Si and SiO 2 with increased activation time is attributed to higher surface roughness and the formation of amorphous layers of Si. While contact angle and surface roughness results show a correlation with bondability, the role of hardness on bondability requires further investigation.