This study presents the change in mechanical and physicochemical behaviour of macrobubbles and sub-millimeter bubbles with respect to pH. While macrobubbles conventionally range from 100 μm to 2 mm in diameter, this study focuses on the comparatively less-explored sub-millimeter bubble range, centered around a median diameter of 500 μm. The difference in sub-millimeter bubbles (500 μm) compared to their larger counterparts (1100 μm) within macrobubble size range were evidenced through atomic force microscopy (AFM) analysis, zeta potential measurements, and rise velocity experiments. The adhesion force and energy between bubbles and the silicon nitride cantilever tip showed a decreasing trend with increasing pH, notably diminishing by about 50% beyond pH 9. Although no significant differences were statistically revealed between the two bubble sizes at lower pH, the adhesion force and energy were consistently smaller for macrobubble compared to sub-millimeter bubble at higher pH beyond pH 9. This finding suggests that the electrical double layer (EDL) interactions are influenced by the specific surface area, particularly in the alkaline region. Zeta potential measurements exhibited a cubic trend, with an isoelectric point at pH 3.5 and a minimum zeta potential at pH 11. The study also depicted a similar trend in the rise velocity of bubbles, suggesting a direct relationship between bubble stiffness and its rise velocity. Therefore, changes in pH affected the bubbles' properties, while on the other hand, certain physicochemical properties are also influenced by bubble sizes.