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ll iScience OPEN ACCESS Figure 6. Charge-discharge voltage profiles of carbon black/Zn electrodes in the saturated solutions of tetramethylammonium chloride at the 5th, 10th, and 30th cycles when different cathode substrate is used (A) Stainless steel foil. (B) Chromium sheet. (C and D) (C) Nickel mesh and (D) Graphite foil. (Figure 7E) corresponds to graphene and Cl-graphene, respectively (Zhao et al., 2015), indicating that the chloride ions absorbed to graphene after the battery fully charge. The corresponding EDS spectrum (Fig- ure 7G) revealed the presence of C, O, and Cl, which imply that some OH groups in GO was substituted by chlorine, and the atomic percentage of C: Cl: O measured by EDS is 73.98:16.54:9.48 and the correspond- ing element weight ratio of C: Cl: O = 63.17:18.35:20.38. The charge and discharge positive carbon materials were characterized by FT-IR and Raman to study the changes of the products during charge and discharge. As shown in Figure 8A, the bands at 3,430 (OH stretching vibration); 3,016 and 2,922 (C-H stretching vibration); 1,488 (C-C stretching); 942 (C-C out-of-plane vibration); and 1,340 (bending vibration) are observed in carbon black cathodes (Luo et al., 2014; Gussoni and Castiqlioni, 2000). When the charge is completed, the bands at 710 cm1 can be clearly observed and attributed to the stretching vibration of C-Cl (Marcus, 2009). However, af- ter the fully discharge, the stretching vibration of C-Cl at 710 cm1 disappeared. This further confirms the chloride ions reversible absorption/desorption in the carbon cathode. In addition, two new peaks of stretching C-O at 1,088 and 1,185 cm1 were also observed after fully charge (Cholpek et al., 2008), indicating that during the charging process, carbon atoms combined with oxygen atoms in the electro- lyte and formed C-O bond. It is noteworthy that only weak intensity of C-Cl bands was observed due to the high absorption coefficient of carbon black in the IR region. Therefore, we further studied the Raman spectrum of graphene in different states. As shown in Figure 8B, there are two dominant peaks at 1,350 cm1 and 1,600 cm1 that correspond to the disordered sp3 hybrid carbon (D band) and crys- talline sp2 hybrid structure (G band) in the Raman spectrum (Liu et al., 2015). The ratio of iD/iG indi- cates the defect degree of the graphene. When the battery fully charged, the ratio of iD/iG is 1.41, which is close to the iD/iG ratio of Cl-Graphene (Kakaei et al., 2016), indicating the existence of Cl-at edges or defects of the graphene during charging process. The iD/iG ratio of graphene decreased to 0.87 when the battery fully discharged, indicating its high-defect degree. It can attribute Article 8 iScience 24, 101976, January 22, 2021PDF Image | aqueous chlorine ion battery
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