Review History


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Summary

  • The initial submission of this article was received on March 12th, 2020 and was peer-reviewed by 3 reviewers and the Academic Editor.
  • The Academic Editor made their initial decision on June 4th, 2020.
  • The first revision was submitted on August 7th, 2020 and was reviewed by 3 reviewers and the Academic Editor.
  • A further revision was submitted on October 28th, 2020 and was reviewed by the Academic Editor.
  • The article was Accepted by the Academic Editor on November 5th, 2020.

Version 0.3 (accepted)

· Nov 5, 2020 · Academic Editor

Accept

The new version is acceptable now.

Version 0.2

· Sep 16, 2020 · Academic Editor

Major Revisions

Two reviewers expressed their concerns about the the formation of co-crystals. If the authors can't provide sufficient evidence to answer the questions, the paper will be rejected.

Reviewer 1 ·

Basic reporting

fair

Experimental design

fair

Validity of the findings

fair

Additional comments

The authors made a lot of changes based on reviewers' comments. However, I found it is still not efficient to support their conclusion.

1. The current results could not support their co-crystal conclusion. The EDS results showed a separation of elements.

2. Why the authors didn't cite their previous paper:
https://pubs.acs.org/doi/10.1021/acsomega.9b03893

Such a small percentage of doped ions changed the XRD patterns dramatically, the authors didn't explain how the transition happens.

Reviewer 2 ·

Basic reporting

I noted that three reviewers have raised doubts about the formation of co-crystals in this work, but it is obvious that the author failed to provide sufficient evidence to support this in the improved version. Therefore, I insist on rejecting this submission.

Experimental design

I noted that three reviewers have raised doubts about the formation of co-crystals in this work, but it is obvious that the author failed to provide sufficient evidence to support this in the improved version. Therefore, I insist on rejecting this submission.

Validity of the findings

I noted that three reviewers have raised doubts about the formation of co-crystals in this work, but it is obvious that the author failed to provide sufficient evidence to support this in the improved version. Therefore, I insist on rejecting this submission.

Additional comments

I noted that three reviewers have raised doubts about the formation of co-crystals in this work, but it is obvious that the author failed to provide sufficient evidence to support this in the improved version. Therefore, I insist on rejecting this submission.

Reviewer 3 ·

Basic reporting

All of my conments have been well answered and this paper can be accepted now.

Experimental design

no comment

Validity of the findings

no comment

Additional comments

All of my conments have been well answered and this paper can be accepted now.

Version 0.1 (original submission)

· Jun 4, 2020 · Academic Editor

Major Revisions

Dear Dr. Nair,
Thank you for your submission to PeerJ Inorganic Chemistry.
It is my opinion as the Academic Editor for your article - Impact of lattice inclusion of Cu and Fe ions on thermal decomposition
characteristics of ammonium perchlorate - that it requires a number of Major Revisions.
My suggested changes and reviewer comments are shown below and on your article 'Overview' screen.

Please address these changes and resubmit. Although not a hard deadline please try to submit your revision within the next 55 days.

[# PeerJ Staff Note: Please ensure that all review comments are addressed in a rebuttal letter and any edits or clarifications mentioned in the letter are also inserted into the revised manuscript where appropriate.  It is a common mistake to address reviewer questions in the rebuttal letter but not in the revised manuscript. If a reviewer raised a question then your readers will probably have the same question so you should ensure that the manuscript can stand alone without the rebuttal letter.  Directions on how to prepare a rebuttal letter can be found at: https://peerj.com/benefits/academic-rebuttal-letters/ #]

Reviewer 1 ·

Basic reporting

no comment

Experimental design

Experimental part is too simple to be a paper. The structure and melting point of the co-crystals should be demonstrated. Please see my comments for the details.

Validity of the findings

The data in the tables were not well explained.

Additional comments

Main logic:
How do you determine it is co-crystal? What are the types of interaction to form co-crystals? Does it affect the melting point or phase transition of the AP? Why the EDS show separation of different elements?
Manuscript preparation:
1. Figure 1, the scale bar is too small. And most of the information under the bottom of the SEM Figures are not necessary, which should be cut off to make them clear.
2. Figure 2, once again, the EDS images should have a scale bar or scale bars are too small to be seen. Also the labeling of elements should be clear and the color of same element from different samples should keep the same to avoid confusing. The original SEM images should be given beside these EDS results.
3. Figure 3, standard AP pattern peaks should be given and marked. The peaks for the doped AP should be assigned.
4. Figure 4, the markers should be hollow to avoid overlapping to each other. Such as, it is hard to distinguish the APFe-1 and APFe-2. DSC data is too overwhelming and the important peaks should be labeled.
5. What method was used for the activation energy calculations? What is the different heating rate when do the calculations? The related information should be given in the main text.
6. How do you know it “in turn improving the ballistic properties of the propellant”? (In abstract and conclusion). Any evidence?
7. Table 1. The mole percentage of Cu or Fe should be given in addition to weight%.
8. Table 1. How did you measure the bulk density and moisture and specific surface area?
9. Please use µm instead of µ when describe the size.
10. Table 2 and Figure 4. Important peaks should be labelled clearly in Figure 4.
11. Line 160, “Copper present in the lattice is the initiation point for LTD and it get oxidized to CuO”, any evidence? Considering the oxidation temperature of Cu, it doesn’t make sense.
12. The authors didn’t talk much about the numbers in their tables.

Reviewer 2 ·

Basic reporting

Less innovative

Experimental design

Less innovative

Validity of the findings

Less innovative

Additional comments

In this manuscript, the authors declared their successful synthesis of two co-crystal compounds incorporating ammonium perchlorate with copper perchlorate or Iron perchlorate. Then the authors studied the impact of the so-prepared materials on thermal decomposition characteristics of ammonium perchlorate. However, the characterization provided in the manuscript obviously cannot evidence the so-prepared materials as co-crystal compounds. Thus, I would reject the manuscript to be published:
(1) The authors provided the SEM images, Elemental mapping and XRD Patterns of Normal AP, ACuP-2 and AFeP-2, which cannot evidence these materials as co-crystal compounds especially the XRD Patterns. I think single-crystal structures and elemental analysis results of these materials are needed.
(2) In abstract, the authors mentioned “the Ammonium perchlorate (AP) is the universal oxidizer in use ... due to ... thermal decomposition without any solid residue”, which is inconsistent with the introduction of copper or Iron ions. Obviously, the solid residue created by copper or iron ions is not welcome in all the solid rocket propellant motors

Reviewer 3 ·

Basic reporting

no comment

Experimental design

no comment

Validity of the findings

no comment

Additional comments

1. In co-crystallisation section, the detailed speed of agitator and cooling rate shoul be added.
2. For better understanding of the physical characteristics of AP, the particle size distribution of AP, AP doped with Cu and Fe should be given like D50 and distribution diagrams.
3. In Line 107, the authors said that the friability of the doped samples are higher compared to normal AP, but there is no evidence and how to prove this.
4. Figure.1 only shows the local SEM images at 10 μm, while single particle of AP, ACuP and AFeP should also be provided for better understanding of whole appearance and size.
5. As listed in Table 1, the weight percent of Cu or Fe is low, however, why is the crystal structure of AP doped with Cu/Fe quite different from normal AP?
6. It is hard to distinguish the line for each sample in Figure 4.
7. Throughout the paper there are many cases that words are either awkward or grammatically incorrect and some are listed below. These confuse the reader and the authors need to check he whole paper carefully.

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