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Photoluminescence (PL) and Fourier‐transform infrared (FTIR) measurements have been performed on light‐emitting porous silicon (LEPSi) after annealing at temperatures below 600 °C. Two different kinds of samples with different surface morphologies and different initial concentrations of chemically bonded hydrogen were studied. In hydrogen‐rich samples we have observed an increase of PL intensity at temperatures up to 250 °C, which correlated with an increase of Si—H bond concentration. A correlation between PL peak wavelength and the ratio of Si—O bonds over Si—H bonds has been demonstrated.