We carefully tailored a porous silicon (pSi) surface by oxidation with hydrogen peroxide (H<sub>2</sub>O<sub>2</sub>) to determine the time-dependent changes in nanocrystallite surface chemistries (e.g., Si-O-Si, SiH<sub>x</sub> [x = 1, 2], O<sub>y</sub>SiH [y = 2, 3], and SiOH/H<sub>2</sub>O) and their influence on the pSi photoluminescence (PL). The relationship between infrared band amplitudes and PL intensity were evaluated under H<sub>2</sub>O<sub>2</sub> and O<sub>3</sub> (previously studied) oxidation. The pSi surface composition under O<sub>3</sub> and H<sub>2</sub>O<sub>2</sub> oxidation conditions tended to, save the O<sub>y</sub>SiH (y = 2, 3) species, approach similar values at the longest oxidation times studied, but they took very different paths in reaching these end points. Furthermore, the pSi surface compositions that exhibit maximum/minimum PL under each oxidant are very different.

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