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In this study, deuterium boride (DB) nanosheets were synthesized as deuterated borophane through the ion exchange of magnesium cations in magnesium diboride with deuterons from a deuterium-type ion-exchange resin in acetonitrile. The Fourier-transform infrared absorption spectrum of DB exhibited clear isotope effects, namely the shift in the absorption peak of the B-H stretching vibrational mode to a lower wavenumber. Temperature-programmed desorption (TPD) from a mixture of DB and hydrogen boride (HB) nanosheets yielded a more intense hydrogen-deuterium (HD) signal compared to the H 2 and D 2 signals. This indicates that the release of hydrogen molecules from the HB nanosheets upon heating originated from interlayer hydrogen recombination rather than intralayer hydrogen recombination. TPD analysis of HB with graphene in different mixing ratios confirmed that the interlayer reaction is predominant in the lower-temperature (<623 K) regime. Meanwhile, the intralayer reaction could proceed in the higher-temperature (>623 K) regime, where hydrogen recombination occurs following H migration on the HB nanosheets.