A broad range of potential applications in numerous industries for silicon nitride (Si3N4) has received extensive attention owing to its intriguing properties such as hardness, high-temperature strength, light weight, large elastic modulus, thermal shock resistance, and electrical resistance. There are numerous methods for generation of silicon nitride such as sol-gel, plasma-assisted hot filament chemical vapor deposition, solid-state reduction-nitridation, nitridation of high-Si-content Fe-Si alloy particles by ammonia (here Fe is a catalyst for NH3 dissociation), 7 thermal-heating chemicalvapor deposition, and catalytic reaction of silicon substrate. Si3N4 nanotube was synthesized before by heating tetraethoxysilane with N2 gas at 165 C. We attempted to synthesize idealized silicon nitride nanotube (SiNNT) in an effort to realize potential materials for hydrogen storage by using the similar synthetic method employed previously for the synthesis of carbon nitride nanotube (CNNT). We prepared SiNNT in a stainless steel autoclave by the reaction of silicon chloride and sodium azide in benzene at 220 C in nitrogen ambient for 15 h. The molar ratio of sodium chloride and sodium azide was 1.0:4.0. We characterized the as-synthesized SiNNT by means of TEM, XPS, XRD, and porosimetry. Figure 1 presents a TEM image of the SiNNT synthesized for 15 h. The nanomaterials turn out to be a hollowed and multi-walled nanotube having a long uniform tubular scaffold. The inner diameters of the nanotubes were measured to be 31.9 ± 7.1 nm. The wall thicknesses were measured to be 11.0 ± 0.3 nm. The nanotubes appear to be end-closed. As presented in Figure 2, we clearly observe the N(1s), Si(2s), and Si(2p) photoelectron emission peaks. The corrected XPS spectral data based on Figures 2(b), 2(c), and the sensitivities of the photoelectron ejections indicate that the as-prepared SiNNT has a stoichiometry of Si:N = 1.000:1.018, the value of which deviates slightly from the theoretical stoichiometry 1.000: 1.3333 for Si3N4. In the present study, we better represent the nanomaterials as SixNy (x = 1.0, y ≈ 1.0) nanotubes. The XRD spectrum as shown in Figure 3 is well matched to the reported SiN crystals. We measured the BET surface area of the nitride nanotube, from which we also