Efficient and Stable Catalytic Hydrogen Evolution of ZrO2/CdSe-DETA Nanocomposites under Visible Light
Round 1
Reviewer 1 Report
The manuscript concerns the synthesis of ZrO2/CdSe-DETA heterojunction materials, that have been investigated as an active photocatalyst in photocatalytic H2 production. In my opinion this manuscript is interesting but it needs major revision before it will be consider for potential publication in Catalysts journal. My reservations and comments are given below.
1. Abstract – Authors should add information on: molar/mass ratio of components in heterjunction materials, the name of the synthesis method that was applied to fabrication those heterjunction.
2. Phare: “specific surface area” should be change to: “BET surface area” or “surface area”.
3. Keywords – should be improve.
4. Introduction – Authors should consider to add information (explanation) on what gave them the introduction of ZrO2 into the photocatalytic material.
5. Lines 56-59 – some information was repeated.
6. Section 2.1. – Authors should add information about temperature of freeze-drying.
7. Lines 82-90 – Authors should consider to add information about the 2 theta values, which are characteristic of the components that build the heterjunction. Moreover, they should also compare the obtained results with those already published. Authors should also calculate the size of the crystallites of the fabricated materials.
8. Figs. 2d-f – Authors should improve description of OX axis. Moreover, Authors should also add information about content of element building of all synthesized materials.
9. Lines 99-106 – Authors should provide the numerical values obtained for EDS analysis for synthesized samples. Moreover, Authors should also compare obtained results with those already published.
10. Lines 120-130 – Are the XPS results consistent with the data that has already been published?
11. Figure 4a – axis OY - phrase “a.u.” should delete. Authors should also present the results of DRS analysis for ZrO2/CdSe-DETA samples.
12. Section 2.5. – Authors should put information about wavelength of characteristic absorption bands for synthesized materials and also compare obtained results with date which were already published.
13. Section 2.6. – Authors should present in Table all information of textural properties of synthesized materials – BET surface area, average pore size and total pore volume.
14. Figure 6a – description of OY axis – should be improve, moreover description of OY axis of figure input should be add. Moreover, in my opinion synthesized materials can’t be classified to mesoporous materials, but hysteresis loop is not visible.
15. Figure 6b – description of four column should be improve.
16. Section 2.7. – Authors should consider to add XRD analysis of sample after photocatalytic tests.
17. Conclusions – should be improve.
18. Supplementary Materials – Section 1.1. – Authors should add information about purity of all used reactants. Could you specify what ZrO2 was used in the study (commercial or self-synthesized)? What is DETA? In what form was Se used in the study, as a metal or as a salt? Please add ethyl alcohol, because it was omitted.
19. Supplementary Materials – Section 1.3. – please add information about preparation of sample for analysis and condition of all used analysis.
20. Supplementary Materials – Section 1.4. – How long the H2 production were performed?
21. I recommend Authors to check the whole manuscript, because there are a lot of editorial mistakes. 22. In my opinion, the authors should consider to add to the manuscript a table which will present the photocatalytic H2 production applying similar materials. 23. All abbreviation which appear in the manuscript should be explained on their first appearance in the text.24. To increase the scientific value of the manuscript Authors should consider extension of the all presented results with comparison of obtained results with the others results described in previous publications.
Author Response
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Author Response File: 
Author Response.pdf
Reviewer 2 Report
The manuscript, titled as “Efficient and stable catalytic hydrogen evolution of ZrO2/CdSe-DETA nanocomposites under visible light”, reported the realization of enhanced hydrogen evolution by novel CdSe-DETA composites. The research was somewhat interesting and could be acceptable after a major revision. Some suggestions were listed as bellow:
1) What was the exact role of EDTA? The sample ZrO2/CdSe should be synthesized and evaluated for photocatalytic performance for comparison;
2) Were mechanisms estimation by calculation and Mott-Schottky plots consistent?
3) The type-I model was generally unfavorable in comparison to other models such as type-II or Z-scheme? Authors should better describe this section to make things more clear to readers;
4) A comparison of such work to previous relevant reports should be made to show the superiority;
5) The structural stability should be provided with relevant supports such as morphological or microstructural analysis.
Author Response
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Author Response File: Author Response.pdf
Reviewer 3 Report
In this manuscript, the authors constructed a type-I ZrO2/CdSe-Diethylenetriamine (ZrO2/CdSe-DETA) hybrid photocatalyst. The ZrO2/CdSe-DETA hybrid photocatalyst exhibits good photocatalytic hydrogen evolution efficiency and durability. The improved photocatalytic performances were attributed to the effective separation of photo-generated electrons. This work is meaningful for developing high photocatalytic activity photocatalysts. Nevertheless, there are several issues that should be addressed.
1、The standard PDF cards of ZrO2 and CdSe should be given in Fig. 1.
2、The change in binding energy of Zr 3d，O 1s，Cd 3d，Se 3d and N 1s should be provided in Fig. 3, and the analysis should be more in-depth rather than only describing the phenomenon.
3、The hydrogen evolution of ZO/CS-0.6 improved at the second and third cycling test in Fig. 7b, while the photocurrent density generally decreased under the light irradiation. Please explain it.
4、Some relative literatures in photocatalytic field including various kinds of photocatalyst should be cited, such as Chin. Chem. Lett. 32 (2021) 2975-2984; J. Alloys Compd. 891 (2021) 161994; Adv. Powder Mater. 2 (2023) 100073; Sep. Purif. Technol., 304 (2023) 122204; Sci. China Chem., 65 (2022) 1704-1709; Chin. J. Catal., 2022, 43, 2652–2664
5、For easier reading, it is suggested that the digital photos of different photocatalysts were displayed in Fig. 4a, which can be referred to: Chem. Eng. J. 412 (2021) 128722; Chem. Eng. J., 452 (2023) 139417.
6、It is better to present the Mott-Schottky plots in the main text.
Author Response
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Author Response File: Author Response.pdf
Round 2
Reviewer 2 Report
It can be accepted in the current form.
