A pyrolysis route has been used to synthesize arrays of highly aligned BxCyNz nanotubes in bulk. The structure and composition of the product were characterized by scanning electron microscopy, high-resolution transmission electron microscopy, and electron energy-loss spectroscopy. The length and diameter of the nanotubes are quite uniform in a large area of the reaction zone. The sizes of the aligned BxCyNz nanotubes from the whole reaction zone are 10–30 μm in length and 20–140 nm in diameter. The x/z ratio of BxCyNz nanotubes for most nanotubes is about 1:1. The x/y ratio of BxCyNz nanotubes is up to 0.6. Within one nanotube, the x/y ratio is usually heterogeneous. The growth mechanism is also discussed.

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