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Nitrogen‐doped single/multi‐walled carbon nanotubes (CNTs) have been studied for a long time from synthesis to properties. However, the stability of N in the CNT lattice still needs further development. In this work, N‐doped double‐walled (DW) CNTs were synthesized using benzylamine as C and N sources. In order to test the stability of N‐doped DWCNTs, high‐temperature annealing in vacuum was performed. By XPS and Raman spectroscopic measurements, we found that the N‐doped DWCNTs are still stable under 1500∘   C  . The amounts of pyrrolic and molecular N decrease after the annealing due to the release effect. However, the amounts of pyridinic and graphitic N greatly increase. Also, the N ratio of the outer tubes increases much more than that of the inner tubes, suggesting that N atoms from the surrounding N‐containing materials combine into the CNT structure during the annealing.

Raman and XPS analyses of pristine and annealed N‐doped double‐walled carbon nanotubes