PONE-D-24-40936PbTe Quantum Dots Highly Packed Monolayer Fabrication by a Spin Coating MethodPLOS ONE

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Reviewer #1: Partly

Reviewer #2: Partly

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Reviewer #1: N/A

Reviewer #2: N/A

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Reviewer #1: Yes

Reviewer #2: Yes

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Reviewer #2: No

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Reviewer #1: Ms. Ref. No.: PONE-D-24-40936 PLOS ONE

Title: PbTe Quantum Dots Highly Packed Monolayer Fabrication by a Spin Coating Method

Comments:

This paper describes the synthesis and characterization of large-area ultrathin layer(s) of PbTe quantum dots(QDs) by the spin coating technique. By optimizing different deposition parameters, the authors claimed that they achieved compact and coherent coating of the large area (~ 3 cm2) substrate with mono/bi-layers of PbTe QDs. This work has made some intriguing and important research progress, but before accepting the manuscript for publication, the authors must address/revise the following issues:

1. In Abstract: The author(s) are advised to avoid vague information and add some key results and numerical findings, mention the type/nature of substrates, processing temperature(s) used for readers. The abstract is detailed but somewhat repetitive, particularly when discussing large-area coating of the underlying substrates, concentrations of coating solutions, etc. Consider condensing the text to avoid redundancy, while still conveying the essential findings.

2. Introduction: Please highlights the motivation behind this study, the novelty of your research, and potential contribution to the literature. There are numerous reports in the literature on PbTe QDs.

(a) The author should justify why they focused on PbTe layer(s) over other important materials, for example, CdTe etc., by highlighting its beneficial optoelectronic features for readers. For example, see Ref1.

Ref.1 Optical Materials 155, 115816, 2024. https://doi.org/10.1016/j.optmat.2024.115816

(b) In lines#42-45, the authors mentioned quantum confinement effect and Bohr excitation radius etc. of materials under study. The authors are advised to elaborate the discussion and provide numerical values of Borh excitation radius for readers with solid first-hand ref(s).

3. Experimental section: (a) Give replace the “Instruments” section at the end. (b) Mention clearly how STEM/TEM specimens of QDs were prepared, which solvents were used for QDs dispersion to be drop-casted on Cu-grid. Also mention the grid size/dimensions for readers. (c) The authors mentioned that they annealed TiO2 thin films grown on ITO/glass substrates at 550C at heating rate of 5C/min, while the glass softening temperature is well below 550C, how they avoid the microcrack of coating layers at such high temperature?

4. Results and Discussions.

(a) In lines#185-189, the authors mentioned the different factors that affect the compact and coherent coating of the substrates of interest. For growing nucleation centers, a clean surface of the desired substrates is a very important factor [Ref.2]. The authors did not mention the cleaning or treatment process of the substrate used. Please clarify this information for the readers.

Ref.1 MRS Advances 8 (5), 194-200, 2023. https://doi.org/10.1557/s43580-023-00515-3

(b) The scale and numerical values in AFM are not legible. Consider the same comments for all relevant images in the manuscript.

(c) In lines#218-226, the authors discovered the substrate surface wetting phenomena by the coating solutions is the crucial factor for coherent and compact layer synthesis. Did the author measure contact angle of the coating solutions/solvents with the substrates used? How author choose suitable solvent(s) for compact layer by spin-coating?

(d) In lines#252-254, the authors wrote, “A tightly packed monolayer of hcp arrays can be detected in this case. The QDs in this layer were highly ordered and monodispersed in their size and shape. However, some amount of surface cracking was identified in the layer.” What did author mean by “hcp arrays”? What was the deposition/processing temperature of thin layer(s)?

(e) Clarify in the Fig. S6. Caption whether images are from S(TEM) images or FE-SEM images.

(f) Correct the Fig. 8 caption, Fig.8c.

(g) Can author include more magnified area-images of PbTe/TiO2 and TiO2/ITO interfaces with SAED for readers.

(h) In lines#430-433, the authors wrote, “The polarity and hydrophobicity of the surface highly influence the fabricated layer. PbTe QDs are known to be hydrophobic,

and for this reason, they create a better layer on hydrophobic TiO2/ITO glass substrate compared to hydrophilic ITO.[56]” The authors are advised to include contact angle of coating solutions/solvents with the substrates of interest to justify this claim.

5. Conclusion: Please re-write the conclusion part again based on the changes that would be made to the current manuscript and highlight the most important factor(s) that play critical role to attain compact and coherent monolayer of PbTe QDs.

Reviewer #2: Manuscript #: PONE-D-24-40936

Title: PbTe Quantum Dots Highly Packed Monolayer Fabrication by a Spin Coating Method

PLOS ONE

Dear Prof. Editor-in-Chief;

The mentioned manuscript subjects to corrections.

1. Polish the English language

2. To improve the manuscript quality, cite for QDs the followings; Quantum Dots: Synthesis, characterization, and optical investigations, IOP Publishing, Bristol, UK. © 2024; Graphene, Nanotubes and Quantum Dots-Based Nanotechnology: Fundamentals and Applications, Elsevier Inc., Netherlands. © 2022; Innovation Discovery 1 (2024) 18-25; Journal of Materials Science: Materials in Electronics 34 (2023) 993-1016; Luminescence 33 (2018) 260-266; Superlattices and Microstructures 88 (2015) 662-667; Canadian Journal of Physics 93 (2015) 1490-1494; Journal of Nanoelectronics and Optoelectronics 10 (2015) 705–710; Materials Science in Semiconductor Processing 39 (2015) 276–282; Solar Energy 115 (2015) 33–39; Renewable Energy 45 (2012) 232-236; Solar Energy 85 (2011) 2283-2287; “Quantum dots-based solar cells for potential application”, in: Mingheng Li (Editor), Energy Systems and Processes: Recent Advances in Design and Control, AIP Publishing, USA. © 2023; “Optical properties of quantum dots”, in: Y. Al-Douri (Editor), Graphene, Nanotubes and Quantum Dots-Based Nanotechnology: Fundamentals and Applications, Elsevier Inc., Netherlands. © 2022

3. Section 2 needs more elaborations

4. Tables 1-2. Any other data for comparison?

5. spherical QDs (6-9 nm) over cubical QDs (10-13 nm). How did you measure?

6. layer with the height of single QD) covering approximately 3 cm². How did you measure

7. Fig. 1. Highlight the thickness

8. Fig. 2. Highlight the grain size

9. QDs monolayer. How did you measure?

10. XRD is required to provide table and structural properties and crystallite size

11. Compare crystallite and grain sizes

12. What’s about optical studies?

13. Pb is a toxic. What’s the safety arrangement to do the experiment?

14. Highlight the advantages of spin coating method

15. Section 4 should reflect abstract

16. 34 of 62 refs is out of date (more than 10 years). Update!

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Reviewer #1: Yes: Syed Farid Uddin Farhad

Reviewer #2: No

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PONE-D-24-40936R1PbTe Quantum Dots Highly Packed Monolayer Fabrication by a Spin Coating MethodPLOS ONE

Dear Dr. Minnes,

Thank you for submitting your manuscript to PLOS ONE. After careful consideration, we feel that it has merit but does not fully meet PLOS ONE’s publication criteria as it currently stands. Therefore, we invite you to submit a revised version of the manuscript that addresses the points raised during the review process.

Please submit your revised manuscript by Feb 06 2025 11:59PM. If you will need more time than this to complete your revisions, please reply to this message or contact the journal office at plosone@plos.org. When you're ready to submit your revision, log on to https://www.editorialmanager.com/pone/ and select the 'Submissions Needing Revision' folder to locate your manuscript file.

Please include the following items when submitting your revised manuscript:

• A rebuttal letter that responds to each point raised by the academic editor and reviewer(s). You should upload this letter as a separate file labeled 'Response to Reviewers'.
• A marked-up copy of your manuscript that highlights changes made to the original version. You should upload this as a separate file labeled 'Revised Manuscript with Track Changes'.
• An unmarked version of your revised paper without tracked changes. You should upload this as a separate file labeled 'Manuscript'.

If you would like to make changes to your financial disclosure, please include your updated statement in your cover letter. Guidelines for resubmitting your figure files are available below the reviewer comments at the end of this letter.

If applicable, we recommend that you deposit your laboratory protocols in protocols.io to enhance the reproducibility of your results. Protocols.io assigns your protocol its own identifier (DOI) so that it can be cited independently in the future. For instructions see: https://journals.plos.org/plosone/s/submission-guidelines#loc-laboratory-protocols. Additionally, PLOS ONE offers an option for publishing peer-reviewed Lab Protocol articles, which describe protocols hosted on protocols.io. Read more information on sharing protocols at https://plos.org/protocols?utm_medium=editorial-email&utm_source=authorletters&utm_campaign=protocols.

We look forward to receiving your revised manuscript.

Kind regards,

María Eugenia Pérez Barthaburu

Academic Editor

PLOS ONE

Journal Requirements:

Please review your reference list to ensure that it is complete and correct. If you have cited papers that have been retracted, please include the rationale for doing so in the manuscript text, or remove these references and replace them with relevant current references. Any changes to the reference list should be mentioned in the rebuttal letter that accompanies your revised manuscript. If you need to cite a retracted article, indicate the article’s retracted status in the References list and also include a citation and full reference for the retraction notice.

Additional Editor Comments:

Thank you for your work on this new version of your manuscript.

Before it can be accepted for publication, I suggest addressing the following points:

1. General Revisions:

Please revise the entire manuscript for grammatical accuracy and clarity.

2. Experimental Details:

Mention how you obtained square QDs. This information is missing both in the experimental description and in Table 1.

3. Specific Edits:

Line 155: Replace the term "purification" with "further cleaning."

4. Ligand Exchange:

In Section 2.4, specify which ligand was exchanged by PDA.

Detail the conditions (e.g., temperature) used during the exchange process.

Explain how you verified that the ligand exchange was successful.

5. Terminology Consistency:

In the abstract, it is stated that round QDs yield better results than cubic ones. However, Section 3 mentions cubic and cuboctahedral QDs. Ensure consistent terminology throughout the manuscript (e.g., rounded/spherical QDs).

6. Structural Adjustments:

The first paragraph of Section 3 (Results and Discussion) should be merged with the Introduction for better flow and coherence.

7. Citations:

Review the citations suggested by Reviewer 2. Retain only the strictly necessary ones, as nearly 10% of the citations are to Al-Douri Y.

8. Figures and Data Presentation:

The images in Figure S1 are unclear. They appear to be in STEM mode within an SEM setup rather than traditional SEM mode. Please clarify and correct this.

Correct the sequence of Figures S4 and S5 in the supplementary information. Since layers of 8.6 nm are mentioned earlier in the manuscript, Figure S5 should precede Figure S4.

Provide details on how the coverage percentage was measured.

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Comments to the Author

1. If the authors have adequately addressed your comments raised in a previous round of review and you feel that this manuscript is now acceptable for publication, you may indicate that here to bypass the “Comments to the Author” section, enter your conflict of interest statement in the “Confidential to Editor” section, and submit your "Accept" recommendation.

Reviewer #2: All comments have been addressed

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6. Review Comments to the Author

Please use the space provided to explain your answers to the questions above. You may also include additional comments for the author, including concerns about dual publication, research ethics, or publication ethics. (Please upload your review as an attachment if it exceeds 20,000 characters)

Reviewer #2: Correct Ref. [6] Journal of Materials Science: Materials in Electronics 34 (2023) 993-1016; Ref. [9] Y. Al-Douri “Quantum dots-based solar cells for potential application”, in: Mingheng Li (Editor), Energy Systems and Processes: Recent Advances in Design and Control, AIP Publishing, USA. © 2023, pp. 6-1–6-18; Ref. [10] Y. Al-Douri (Editor), Graphene, Nanotubes and Quantum Dots-Based Nanotechnology: Fundamentals and Applications, Elsevier Inc., Netherlands. © 2022; Ref. [15] Y. Al-Douri (Author), Quantum Dots: Synthesis, characterization, and optical investigations, IOP Publishing, Bristol, UK. © 2024; Ref. [26] correct: Renewable Energy

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Do you want your identity to be public for this peer review? For information about this choice, including consent withdrawal, please see our Privacy Policy.

Reviewer #2: No

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PbTe Quantum Dots Highly Packed Monolayer Fabrication by a Spin Coating Method

PONE-D-24-40936R2

Dear Dr. Minnes,

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Kind regards,

María Eugenia Pérez Barthaburu

Academic Editor

PLOS ONE

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