In Situ Electroplating of Ir@Carbon Cloth as High-Performance Selective Oxygen Evolution Reaction Catalyst for Direct Electrolytic Recovery of Lead
Round 1
Reviewer 1 Report
The authors reported that a simple electrodeposition method was used to fabricate the Ir catalyst on the pretreated CC surface. The optimized catalyst exhibited an overpotential of 256 mV for OER in MSA solution with a longer lifetime and better catalytic stability than Ir/C. Moreover, the catalyst can be used as the anodic catalyst for recovery Pb from lead methanesulfonate electrolyte. The design of this experiment has a certain novelty. However, there are still some unclear aspects on the details of experiment and mechanism of this work. Specifically, there are several deficiencies:
(1) The electron transport of catalyst is not only in the high frequency region, please refer to the literatures (J. Am. Chem. Soc. 2019, 141, 3014-3023 and Nano Energy 2022, 104,107960) for analysis.
(2) The author needs to explain why the solution resistance (Rs) of Ir/C catalyst is much greater than that of other catalysts.
(3) The author needs to further analyze and summarize why the CC-Ir catalyst has better performance.
(4) Faraday efficiency needs to be tested.
(5) Why does the XRD pattern of only CC-3 show obvious peaks of metallic iridium.
(6) Has the author investigated how to separate and reuse the catalyst since PbO2 is grown on the surface of the CC-Ir electrode.
Author Response
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Reviewer 2 Report
Report on the manuscript catalysts-2165583 entitled “In situ Electroplating of Ir@ carbon cloth as high performance Selectively Oxygen Evolution Reaction Catalyst for Direct electrolytic recovery of lead”.
The submitted manuscript should be revised. The following points should be addressed:
1. The submitted manuscript should be revised to be free from editing or grammar errors.
2. The mapping of oxygen is not clear in figures 2 and 6.
3. All mentioned XRD cards should be combined with references.
4. In XPS analysis, the oxygen wasn’t studied even in deconvoluted fitting or discussion in manuscript and it has a valuable content as appeared in Fig. 3A.
5. Equivalent circuit analysis should be studied by impedance analysis [suggested reference to study it: Journal of Alloys and Compounds, Volume 816, 2020, 152513].
Author Response
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Reviewer 3 Report
Comments are attached
Comments for author File: 
Comments.pdf
Author Response
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Reviewer 4 Report
In this manuscript, the authors used a simple plating method to prepare Ir-based catalysts on CC surfaces for the electrolytic recovery of lead. The nano-CC-Ir with an Ir loading of 7.2% was obtained by adjusting the optimal current density, plating temperature, and plating time. The material has a low overpotential (256 mV), better stability, and better electrochemical performance than commercial Ir/C catalysts in 0.5 M methanesulfonic acid solution. In the electrolytic recovery of lead, CC-Ir has an inhibitory effect on PbO2 side reactions and can improve the lead recovery rate. This manuscript will provide an unusual perspective to profoundly understand and inspire the design of advanced catalysts for the electrolytic recovery of lead. Therefore, I would recommend the acceptance of this manuscript after minor revision as the following:
1. “Pretreatment and Electroplate” should be changed to “Pretreatment and Electroplating” in Figure 1.
2. The author should add the space between the coordinate name and the parentheses, such as in Figure 3a.
3. Generally, EDS is not accurate in measuring elemental content. It is suggested to check the mass fraction of Ir by the accurate way, for example, ICP-AES.
4. XPS spectra of Ir4f in Figure 3d and O1s in Figure 6e should be fitted well. We can observe that the original data (grey line) and fitted curve (red line) are not matched well.
Author Response
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Round 2
Reviewer 1 Report
It can be accepted by Catalysts.
Reviewer 2 Report
The revised version of the manuscript could be accepted.
