Through the XRD characterization of the three materials, a distinctive diffraction peak appears near 20°, as illustrated in
Figure 3
c. Comparison with the PDF card, the characteristic peak suggested the presence of certain carbon material composition in the three materials [
31
]. The introduction of nZVI and CTS did not alter the structure and composition of the original biological carbon. No significant deviation was observed in the characteristic peaks of nZV-WSPC and CTS@nZVI-WSPC, indicating a minimal difference in their crystal structure. This is attributed to the fact that CTS acts as a natural polymer polysaccharide, with characteristic diffraction peaks predominantly occurring at 10–20°. The appearance of this characteristic peak is a result of intermolecular or intramolecular hydrogen bonds stemming from the presence of -OH and -NH
2
functional groups in CTS [
32
,
33
]. Many salts or oxides tend to disperse on the carrier surface to form monolayers and submonolayers. In the case where the loading amount is below a certain threshold, a monolayer dispersion state is maintained, and the active component cannot be detected by X-ray. From the XRD profile, it is evident that nZVI was successfully synthesized in both composites. The diffraction peaks are located at 30.27°, 35.68°, 44.5°, 57.4°, and 63.25°, corresponding to different forms of iron (Fe), with the peaks at 44.5° and 63.25° specifically indicating the presence of nano-zero-valent iron, as reported in various literature sources [
34
]. Moreover, the diffraction peaks of CTS@nZVI-WSPC at 2θ = 29.9°, 40.17°, and 55.08° align well with the ferric oxide standard card, which appears after the adsorption reaction [
35
,
36
]. The characteristic peak band at 35.19° represents the formation of ferric oxide, suggesting that the composite may undergo oxidation after the reduction by iron particles, which is consistent with the XPS analysis results. The comprehensive analysis showed that the introduction of nZVI and chitosan did not alter the carbon structure of the raw wheat straw. After the reaction, the material’s structure remained largely unchanged, retaining a stable morphology.