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Recently, electrolytic zinc\u2010manganese batteries, exhibiting the pure dissolution\u2010deposition behavior with a large charge capacity, have been accomplished through using electrolytes with Lewis acid. However, the complicated chemical environment and mixed products hinder the investigation though it is crucial to understand the detailed mechanism. Here, cyclic voltammetry coupled electrochemical quartz crystal microbalance (EQCM) and ultraviolet\u2010visible spectrophotometry (UV\u2013Vis) are respectively, for the very first time, used to study the transition from zinc\u2010ion batteries to zinc electrolytic batteries by the continuous addition of acetate ions. These complementary techniques operando trace the mass and the composition evolution. The observed formation and dissolution of zinc hydroxide sulfate (ZHS) and manganese oxides evince the effect of acetate ions on zinc\u2010manganese batteries from an alternative perspective. Both the amount of acetate and the pH value have large impacts on the capacity and Coulombic efficiency of the MnO<jats:sub>2<\/jats:sub> electrode, and thus they should be optimized when constructing a full zinc\u2010manganese battery with high rate capability and reversibility.<\/jats:p>","DOI":"10.1002\/cssc.202300259","type":"journal-article","created":{"date-parts":[[2023,3,4]],"date-time":"2023-03-04T05:35:35Z","timestamp":1677908135000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":13,"title":["Complementary Operando Electrochemical Quartz Crystal Microbalance and UV\/Vis Spectroscopic Studies: Acetate Effects on Zinc\u2010Manganese Batteries"],"prefix":"10.1002","volume":"16","author":[{"given":"Zi\u2010Fan","family":"He","sequence":"first","affiliation":[{"name":"Department of Chemical Engineering National Tsing Hua University  Hsin-Chu 300044 Taiwan"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-2128-1385","authenticated-orcid":false,"given":"Yi\u2010Ting","family":"Lu","sequence":"additional","affiliation":[{"name":"Department of Chemical Engineering National Tsing Hua University  Hsin-Chu 300044 Taiwan"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-9608-8275","authenticated-orcid":false,"given":"Tzu\u2010Chien","family":"Wei","sequence":"additional","affiliation":[{"name":"Department of Chemical Engineering National Tsing Hua University  Hsin-Chu 300044 Taiwan"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-4308-8474","authenticated-orcid":false,"given":"Chi\u2010Chang","family":"Hu","sequence":"additional","affiliation":[{"name":"Department of Chemical Engineering National Tsing Hua University  Hsin-Chu 300044 Taiwan"}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"311","published-online":{"date-parts":[[2023,4,18]]},"reference":[{"key":"e_1_2_8_1_1","unstructured":"\u00a0"},{"key":"e_1_2_8_2_2","doi-asserted-by":"publisher","DOI":"10.1002\/aenm.201901968"},{"key":"e_1_2_8_3_2","doi-asserted-by":"publisher","DOI":"10.1016\/j.nanoen.2019.05.059"},{"key":"e_1_2_8_4_2","doi-asserted-by":"publisher","DOI":"10.1016\/j.joule.2020.03.002"},{"key":"e_1_2_8_5_2","doi-asserted-by":"publisher","DOI":"10.1021\/acs.chemmater.8b03409"},{"key":"e_1_2_8_6_2","doi-asserted-by":"publisher","DOI":"10.3389\/fenrg.2020.602918"},{"key":"e_1_2_8_7_1","unstructured":"\u00a0"},{"key":"e_1_2_8_8_2","first-page":"265","volume":"4","author":"Linden D.","year":"1995","journal-title":"Fuel Energy Abstr."},{"key":"e_1_2_8_9_2","doi-asserted-by":"publisher","DOI":"10.1021\/cr020730k"},{"key":"e_1_2_8_10_2","first-page":"141","volume":"5","author":"Kuchhal P.","year":"2019","journal-title":"Environ. 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