The observed difference in the Raman spectra can be used to distinguish between short and long sulfur chains in S/DIB copolymers, for example in the synthesis process or during cycling of the battery. To validate the above theoretical observation, first five S/DIB copolymers are synthesized with different mass fractions of DIB (and consequently varying S chain lengths) using inverse vulcanization. Here, we refer to them as SDIBw in which w is the wt % of DIB, namely 20, 25, 30, 40, and 50%. These mass fractions correspond stoichiometrically to average chain lengths of 11, 8, 6, 4, and 3 sulfur atoms, respectively. Presence of the connection between S chains and DIB molecules is confirmed in all synthesited samples by liquid-state NMR spectroscopy while crystal formation is ruled out by X-ray diffraction measurements (see the Supplementary Information). In a second step, Raman spectra of the synthesized sulfur copolymers are measured. normalized with respect to that of the peak at ∼1000 cm -1 in SDIB20 sample. This peak is present in all Raman spectra and corresponds to an aromatic ring vibration. The Raman peak for the characteristic S-S stretching is observed at 473 cm -1 , which is about 4% higher than the theoretically predicted value. The presence of peaks in 1560-1640 cm -1 region indicates partially unsaturated propenyl groups. It is observed that these peaks become more intensive with increasing w. This is in agreement with our NMR measurements (see Sup- In addition, in Fig. we observe Raman activities at ∼165-200 cm -1 assigned to the sulfur chain deformation and S-S-S bending [see Fig. (a) and (b)], which gradually disappear with increasing wt % of DIB (shorter sulfur chains).