Figure
2 provides the x-ray diffraction (XRD), Raman and x-ray photoelectron spectroscopy (XPS) spectra, complex permittivity, and reflection loss (RL) results of CCBNFs-1, CCBNFs-2, and CCBNFs-3. As shown in Fig.
2A, CCBNFs-1, CCBNFs-2, and CCBNFs-3 exhibit the (002) and (100) characteristic diffraction peaks corresponding to carbon [
28]. With the carbonization temperature increasing from 700 to 900 °C, the (002) peak position gradually shifts from 24.4° to 24.9°. The shift of peak position toward the positive direction indicates that elevated temperature promotes the transformation of amorphous carbon toward graphitization [
29]. The characteristic peaks (Fig.
2B) at ca. 1,348 cm
−1 (D peak) representing the disordered carbon structure and 1,582 cm
−1 (G peak) corresponding to graphitized carbon are observed over CCBNFs-1, CCBNFs-2, and CCBNFs-3. The
ratio gradually decreases from 1.08 (CCBNFs-1) to 1.03 (CCBNFs-2) and 0.99 (CCBNFs-3), which further confirm the gradual enhancement of graphitized degree for obtained samples [
30]. To further determine the chemical composition, XPS characterization was performed. As shown in Fig.
2C, all the acquired mesoporous carbon HNSs@carbon BNFs show the obvious C 1s, N 1s, and O 1s characteristic peaks. It is worth noting that the intensity of N 1s peak for mesoporous carbon HNSs@carbon BNFs gradually decreases by increasing the carbonization temperature, indicating a decreased trend of N content caused by the volatilization or decomposition of N under high-temperature conditions [
31]. In addition, the high-resolution XPS spectra of C 1s (Fig.
2D) can be fitted by C–C/C=C (283.2 eV), C=N (284.5 eV), C–N (284.9 eV), and O–C=O (288.8 eV) bonds [
32,
33]. As given in Fig.
2E, the C–C/C=C content in the obtained sample is also gradually increased from CCBNFs-1 to CCBNFs-2 and CCBNFs-3, which is also consistent with the XRD and Raman results. The enhancement of graphitization favorably contributes to the enhancement of electrical conductivity [
34]. Additionally, the obtained mesoporous carbon HNSs@carbon BNFs present the decreased C=N bond content and a slight enhanced C–N and O–C=O bond contents, which is due to the partial breakage and rearrangement of C=N bond at high temperatures. This facilitates the enhancement of structural ordering and manifests as a slight rightward shift in the overall peak position [
35]. As provided in Fig.
2F, the high-resolution N 1s XPS spectra of CCBNFs-1, CCBNFs-2, and CCBNFs-3 show a decreasing trend in N content. The N 1s spectra are deconvoluted into 4 typical nitrogen configurations: pyrrole nitrogen (~396.7 eV), pyridine nitrogen (~397.9 eV), graphitic nitrogen (~399.3 eV), and nitrogen oxide (402.0 eV) [
36]. The quantitative analysis results (Fig.
2G) show that the obtained mesoporous carbon HNSs@carbon BNFs present gradually increased contents of graphite nitrogen and nitrogen oxide by increasing the carbonization temperature. According to the previous results [
37], the enhancement of graphitic nitrogen can enhance the
sp2 conjugated network of carbon skeleton, which is conducive to optimize the electrical conductivity. In summary, XRD, Raman, and XPS results indicate that precise temperature control enables microscopic regulation of nitrogen doping concentration and crystallinity. As shown in Fig.
2H and I, owing to the intrinsic properties of carbon materials and their hollow structures, the obtained fibers exhibit high complex permittivity values even at a low filling ratio of 12.5%. The complex permittivity (
) values of CCBNFs-1, CCBNFs-2, and CCBNFs-3 show a decreasing trend within 2 to 18 GHz, which are in agreement with the Debye theory. In addition, both
(Fig.
2H) and
(Fig.
2I) show a pattern of CCBNFs-1 < CCBNFs-2 < CCBNFs-3, which implies the enhanced electrical conductivity [
38]. Compared with mesoporous carbon HNSs@carbon BNFs, the SiO
2/carbon SNSs@PAN BNFs exhibit the relatively low
and
values (Fig. S2A) owing to the presence of silica and solid structure. The obtained complex permittivity results are consistent with the XRD, Raman, and XPS findings. As shown in the 2D RL diagrams for CCBNFs-1 (Fig.
2J), CCBNFs-2 (Fig.
2K), CCBNFs-3 (Fig.
2L), and SiO₂/carbon SNSs@PAN BNFs (Fig. S2B), CCBNFs-2 exhibits a superior EAB value. To further investigate variations in its MAPs, Fig.
2M provides the 2D RL plots of CCBNFs-1, CCBNFs-2, and CCBNFs-3, which have an RL
min value of −15.45 dB at 13.6 GHz, −21.18 dB at 2.8 GHz, and −65.82 dB at 5.8 GHz. Their corresponding
dm values of RL
min values are 10.00, 9.77, and 4.72 mm. Furthermore, the EAB values of CCBNFs-1 (Fig.
2J), CCBNFs-2 (Fig.
2K), and CCBNFs-3 (Fig.
2L) are 2.60 GHz at 8.32 mm (15.4 to 18 GHz), 4.60 GHz at 2.24 mm (13.2 to 17.8 GHz), and 3.40 GHz at 1.87 mm (14.6 to 18 GHz), respectively.