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Article
Peer-Review Record

Preparation of Melamine Formaldehyde Foam and a Melamine-Formaldehyde-Organo-Clay Nanocomposite and Hybrid Composites

Minerals 2023, 13(11), 1407; https://doi.org/10.3390/min13111407
by Ahmet Gürses 1,* and Elif Şahin 2
Reviewer 1: Anonymous
Reviewer 2: Anonymous
Reviewer 3: Anonymous
Reviewer 4: Anonymous
Minerals 2023, 13(11), 1407; https://doi.org/10.3390/min13111407
Submission received: 5 September 2023 / Revised: 30 October 2023 / Accepted: 31 October 2023 / Published: 2 November 2023

Round 1

Reviewer 1 Report

Comments and Suggestions for Authors

Comments:

1. The title is too long and complicated.

2. What are the differencees between melamine formaldehyde-organo-clay nanocomposite and some hybrid composites?

3. The abstract and introduction of this manuscript should be rearranged in  a more concise way.

4. "Kaolin" clay should be "Kaolin", while "Montmorillonite clay" should be "Montmorillonite".

5. "The mineralogical composition" should be "The XRF chemical composition". Similarly hereinafter.

6. "oC" should be "°C".

7. It is difficult to observe the 2:1 layered structure from Figure 1.

8. Please replace the full names of the samples with the corresponding abbreviations.

9. Please retest the FTIR spectra of the relevant samples.

10. Please provide the unit of "°" for all the numbers of diffraction peaks.

11. " characteristic peaks of kaolin" should be "characteristic peaks of kaolinite". In fact, "kaolin" should be "kaolinite", please differentiate the difference and relationship of them.

Comments on the Quality of English Language

The language should be more concise and polished.

Author Response

Responses to Ref 1

We are grateful to the Reviewer for   very helpful suggestions. In the light of these suggestions, the manuscript was reviewed throughout and the necessary revisions were made. The corrections are highlighted in red on the text. In addition, the answers to the referee suggestions are also given one by one.

 

  1. The title is too long and complicated.

It was changed as “Preparation of melamine formaldehyde foam and melamine formaldehyde-organo-clay nanocomposite and hybrid composites”

  1. What are the differences between melamine formaldehyde-organo-clay nanocomposite and some hybrid composites?

The most obvious difference between melamine formaldehyde nano composite and hybrid composites is the content, composition and dispersion characteristics. Primary additive, a higher amount of mineral matrix, and a secondary additive, a lower amount of mineral reinforcement, were added to the nano composite with lower mechanical strength. Thus, It is aimed to prepare hybrid composites with higher mechanical strength. However, nanocomposites are sometimes called hybrid composites.

 

  1. The abstract and introduction of this manuscript should be rearranged in  a more concise way.

They have been concisely revised.

  1. "Kaolin" clay should be "Kaolin", while "Montmorillonite clay" should be "Montmorillonite".

It was made.

  1. "The mineralogical composition" should be "The XRF chemical composition". Similarly hereinafter.

It was made.

  1. "oC" should be "°C".

It was made.

  1. It is difficult to observe the 2:1 layered structure from Figure 1.

At first glance, the referee may be right, but as the size is increased, the structure can be observed more clearly. Even in its current form, it can be said that the fibrous patterns can reflect the layered structure quite well.

 

  1. Please replace the full names of the samples with the corresponding abbreviations.

Since the abbreviations were defined at the beginning, the examples are referred to with abbreviations in order not to lengthen the text, but often full names are also used.

  1. Please retest the FTIR spectra of the relevant samples.

The referee may be right, but the individual spectra look much more detailed. As a result of the display together, a decrease in peak intensity occurs. However, an attempt has been made to visualize this with numerical representation.

  1. Please provide the unit of "°" for all the numbers of diffraction peaks.

It was made.

  1. " characteristic peaks of kaolin" should be "characteristic peaks of kaolinite". In fact, "kaolin" should be "kaolinite", please differentiate the difference and relationship of them.

It was corrected

Author Response File: Author Response.docx

Reviewer 2 Report

Comments and Suggestions for Authors

-Please include details about the experimental processes in the abstract section. It would be more striking to include more analysis results numerically.

 

It would be more meaningful if the improvement in thermal conductivity or glass transition temperatures were emphasized in the abstract section.

 

-In general, it is recommended to include literature findings from the last 5 years in the manuscript

 

-In the introduction section, please explain the outstanding feature of this research by giving examples of mechanical and thermal properties of current research.

 

-please specify the surface areas of the clays used in the material section

 

-Correct the temperature values in the manuscript. B was prepared at 40oC by....the degree symbol should be given as superscript. Check all units, FTIR is also cm-1??? should be superscript

 

-Please indicate the magnification rates of the morphological surface in SEM analysis in the text.

 

-Please interpret intercalation and exfoliation structures separately for composite and organoclay and state their importance.

It will be useful for you to benefit from the following article.

Investigation of Antimicrobial Properties of QASs+ (Novel Synthesis)

G Baysal, H Aydın, S Uzan, H HoÅŸgören

Russian Journal of Physical Chemistry B 12, 695-700

-A comparison with the literature will make the results section more impressive.

Author Response

Responses to Ref 2

We are grateful to the Reviewer for   very helpful suggestions. In the light of these suggestions, the manuscript was reviewed throughout and the necessary revisions were made. The corrections are highlighted in red on the text. In addition, the answers to the referee suggestions are also given one by one.

-Please include details about the experimental processes in the abstract section. It would be more striking to include more analysis results numerically.

It was made

It would be more meaningful if the improvement in thermal conductivity or glass transition temperatures were emphasized in the abstract section.

It was made

 -In general, it is recommended to include literature findings from the last 5 years in the manuscript

 The referee may be right, but the reference list is quite extensive.

-In the introduction section, please explain the outstanding feature of this research by giving examples of mechanical and thermal properties of current research.

It was revised

-please specify the surface areas of the clays used in the material section

They were added.

 -Correct the temperature values in the manuscript. B was prepared at 40oC by....the degree symbol should be given as superscript. Check all units, FTIR is also cm-1??? should be superscript

They were corrected.

 -Please indicate the magnification rates of the morphological surface in SEM analysis in the text.

They do not appear together due to presentation

 -Please interpret intercalation and exfoliation structures separately for composite and organoclay and state their importance.

It was made.

It will be useful for you to benefit from the following article.

Investigation of Antimicrobial Properties of QASs+ (Novel Synthesis)

G Baysal, H Aydın, S Uzan, H HoÅŸgören

Russian Journal of Physical Chemistry B 12, 695-700

Thanks for the suggestion. It is cited in the appropriate place.

-A comparison with the literature will make the results section more impressive.

It was made

Author Response File: Author Response.docx

Reviewer 3 Report

Comments and Suggestions for Authors

The authors make an extensive study on the preparation of MF polymers with a series of fillers, classified in 3 classes: OMMT, primary, and secondary.

Several issues should be improved:

*Abstract: OMMT is not mentioned as a filler in lines 15-18. Why? Moreover, the abstract is too long and contains too many experimental details. It should be shortened, some parts should be deleted or moved to the conclusion (see below).

* It is not clear what the role of OMMT in such low amounts (only 0.11%) would be.  Also, it should be difficult to characterize, identify them in the composite.

*line 289: please write clay "platelets", not "grains"

*Section 3.2: it is difficult to follow the argument of the authors, as the images are not very clear. Are these SEM images from fractured surfaces, or from the original surface? The authors mention "clusters of microspheres", "branched structures", "spherical polymer clay NCs", "porous pumice plates", etc, but it is difficult to identify them in the images (Fig. 3). The authors should mark these elements in the images. Moreover, please make the scale bar more legible. What are the holes in Fig. 3?

* Figure 4: The curve for MF should be expanded vertically to look similar to the other ones. The peaks cannot be seen, the authors should mark them. Moreover, the axes should also have a title, not only the units.

* Fig. 4 and 5: why do the authors expect a change in the curves for so low amounts of OMMT (0.11%)?

* Figure 5: add axes titles.

* Conclusion: there is no conclusion, the authors should add one.

 

 

Author Response

Responses to Ref 3

We are grateful to the Reviewer for   very helpful suggestions. In the light of these suggestions, the manuscript was reviewed throughout and the necessary revisions were made. The corrections are highlighted in red on the text. In addition, the answers to the referee suggestions are also given one by one.

 

The authors make an extensive study on the preparation of MF polymers with a series of fillers, classified in 3 classes: OMMT, primary, and secondary.

Several issues should be improved:

*Abstract: OMMT is not mentioned as a filler in lines 15-18. Why? Moreover, the abstract is too long and contains too many experimental details. It should be shortened, some parts should be deleted or moved to the conclusion (see below).

Abstract has been concisely revised.

Organo Montmorillonite (OMMT) could be specified as a reinforcement or nano material/filler. It is not referred to as a typical filler at microscopic size.

* It is not clear what the role of OMMT in such low amounts (only 0.11%) would be.  Also, it should be difficult to characterize, identify them in the composite.

The referee may be right, but as it is known, nano additives can provide superior properties to the material when used in very low amounts. This is one of the reasons why it is not mentioned as a filler. Preliminary tests have shown that even amounts below 1% can provide significant improvements in many properties of the material.

*line 289: please write clay "platelets", not "grains"

Thanks to the referee. It has been corrected.

*Section 3.2: it is difficult to follow the argument of the authors, as the images are not very clear. Are these SEM images from fractured surfaces, or from the original surface? The authors mention "clusters of microspheres", "branched structures", "spherical polymer clay NCs", "porous pumice plates", etc, but it is difficult to identify them in the images (Fig. 3). The authors should mark these elements in the images. Moreover, please make the scale bar more legible. What are the holes in Fig. 3?

SEM images were taken from powder samples. When the figure is enlarged, it is clear that the depiction becomes more observable due to the increased clarity. Since the polymeric matrix is prepared in foam form, the holes indicate possible air gaps.

* Figure 4: The curve for MF should be expanded vertically to look similar to the other ones. The peaks cannot be seen; the authors should mark them. Moreover, the axes should also have a title, not only the units.

They were made

* Fig. 4 and 5: why do the authors expect a change in the curves for so low amounts of OMMT (0.11%)?

Thank you for your attention. A correction was made in the calculation and the organo-clay ratio was changed to 0.15. In addition, a systematic analysis of the organo-clay ratio was made and it was determined that the increase did not cause much significant change. As seen in the experimental results, this ratio caused significant positive changes in most samples.

* Figure 5: add axes titles.

* Conclusion: there is no conclusion, the authors should add one.

It was added.

Author Response File: Author Response.docx

Reviewer 4 Report

Comments and Suggestions for Authors

The manuscript entitled "Investigation of texture, thermal conduction and some mechanical properties of melamine formaldehyde foam and melamine formaldehyde-organo-clay nanocomposite and some hybrid  composites" presents interesting results but needs substantial improvement before it can be considered for publication in Minerals, as I can list some of them below:

1. The abstract is too long and contains a quite long unnecessary explanation such as the Experimental part. Basically, the abstract must be able to stand alone. The authors must rewrite this part and add more important results in this section.

2. There is no structure in the Introduction part except the long text. Therefore, it needs to be improved and restructured to show better the work's originality and importance. Moreover, it seems that the novelty of the work with respect to the literature, and the state of the art are not well highlighted in the paper.

3. I highly recommend rewriting some parts of the introduction and giving some examples of using non-modified and modified MMT nanoparticles in weak bioplastic matrices and reporting their substantial effects on the mechanical properties of composites. For this purpose, you can use the following reference: https://doi.org/10.3390/ma16030900.

4. It is highly recommended to merge Tables 1, 2, and 3. Moreover, Table 8 needs to be improved and should be moved to section 2.2.2.

5. Please, improve the quality of the figures, in particular, Figure 5 by separating the curves   

6. The manuscript does not have a conclusion section. It should be well drawn from the results.

7. The mechanical properties and thermal conductivity values should be presented in a table along with the standard deviations that it is an important feature of the work.

8. The author did not show any mechanical properties results of melamine formaldehyde (MF) as the benchmark for better comparison. In this regard, adding the result of this sample is highly recommended.

9. Let the table and figure legends be more informative (especially abbreviations and sample codes) to avoid the readers getting back to the methodology section to understand what we can see in the results.

10. There are many grammatical errors. Please have a thorough proofread of the entire manuscript for proper English usage.

Comments on the Quality of English Language

There are many grammatical errors. Please have a thorough proofread of the entire manuscript for proper English usage.

Author Response

Responses to Ref 4

We are grateful to the Reviewer for   very helpful suggestions. In the light of these suggestions, the manuscript was reviewed throughout and the necessary revisions were made. The corrections are highlighted in red on the text. In addition, the answers to the referee suggestions are also given one by one.

 

The manuscript entitled "Investigation of texture, thermal conduction and some mechanical properties of melamine formaldehyde foam and melamine formaldehyde-organo-clay nanocomposite and some hybrid composites" presents interesting results but needs substantial improvement before it can be considered for publication in Minerals, as I can list some of them below:

  1. The abstract is too long and contains a quite long unnecessary explanation such as the Experimental part. Basically, the abstract must be able to stand alone. The authors must rewrite this part and add more important results in this section.

Abstract has been concisely revised.

 

  1. There is no structure in the Introduction part except the long text. Therefore, it needs to be improved and restructured to show better the work's originality and importance. Moreover, it seems that the novelty of the work with respect to the literature, and the state of the art are not well highlighted in the paper.

It was concisely revised.

  1. I highly recommend rewriting some parts of the introduction and giving some examples of using non-modified and modified MMT nanoparticles in weak bioplastic matrices and reporting their substantial effects on the mechanical properties of composites. For this purpose, you can use the following reference: https://doi.org/10.3390/ma16030900.

Thanks for the suggestion. It was gladly taken into consideration.

  1. It is highly recommended to merge Tables 1, 2, and 3. Moreover, Table 8 needs to be improved and should be moved to section 2.2.

Thanks to the referee for his very sound suggestions. They have been made.

  1. Please, improve the quality of the figures, in particular, Figure 5 by separating the curves 

They were made

  1. The manuscript does not have a conclusion section. It should be well drawn from the results.

It was added

  1. The mechanical properties and thermal conductivity values should be presented in a table along with the standard deviations that it is an important feature of the work.

Thanks so much for the reminder. It's done.

  1. The author did not show any mechanical properties results of melamine formaldehyde (MF) as the benchmark for better comparison. In this regard, adding the result of this sample is highly recommended.

The referee may be right, but since it is prepared in foam form, it is too brittle a material to be suitable for the mentioned tests.

  1. Let the table and figure legends be more informative (especially abbreviations and sample codes) to avoid the readers getting back to the methodology section to understand what we can see in the results.

They were revised.

  1. There are many grammatical errors. Please have a thorough proofread of the entire manuscript for proper English usage.

The manuscript has been thoroughly reviewed in this context.

Author Response File: Author Response.docx

Round 2

Reviewer 1 Report

Comments and Suggestions for Authors

This manuscript can be accepted for publication after revision some errors, and the conclusions should be sumarried instead of stating point by point. For example, Line 213: "95oC" should be "95oC".; Line 288: "From Fig 2a it can be seen that......" should be "From Fig 2a, it can be seen that......"; Line 320: "Figure 3c" should be "Fig 3c"; etc. 

 

Comments on the Quality of English Language

The language should be polished in a concise way, especially Abatract, Introduction and Conclusions.

Author Response

Responses to Referee 1

 

This manuscript can be accepted for publication after revision some errors, and the conclusions should be sumarried instead of stating point by point. For example, Line 213: "95oC" should be "95oC".; Line 288: "From Fig 2a it can be seen that......" should be "From Fig 2a, it can be seen that......"; Line 320: "Figure 3c" should be "Fig 3c"; etc. 

Thank you very much for the useful corrections.

They are made.

Author Response File: Author Response.docx

Reviewer 3 Report

Comments and Suggestions for Authors

The authors performed the required corrections. The manuscript can be now accepted for publication.

Author Response

Responses to Referee 2

The authors performed the required corrections. The manuscript can be now accepted for publication.

Thank you very much

Reviewer 4 Report

Comments and Suggestions for Authors

The authors have done a good job in revisiting the manuscript and making it better by answering most of the queries raised. Thus, I recommend the acceptance of the manuscript for publication in Minerals after addressing the below-mentioned comments:

1. I think the abstract is still long and unnecessary explanations like the experimental text should be omitted (Lines 21-25).

2. As I stated in the last review report, Table 3 should be moved to section 2.2.2.

3. There are two errors in the numbering of the references. The numbers 53 and 54 are repeated for the related references.

 

4. Authors must indicate clearly observed differences in the wavenumbers of peaks in the FT-IR spectra (Figure 4) with the bar line and still the quality of the figure needs to be improved. For example, the authors can simply use the horizontal legend, or delete the legends and insert the sample codes on each curve.

Comments on the Quality of English Language

Minor editing of English language required

Author Response

Responses to Referee 4

Thank you very much for the useful corrections.

The authors have done a good job in revisiting the manuscript and making it better by answering most of the queries raised. Thus, I recommend the acceptance of the manuscript for publication in Minerals after addressing the below-mentioned comments:

  1. I think the abstract is still long and unnecessary explanations like the experimental text should be omitted (Lines 21-25).

It was made.

  1. As I stated in the last review report, Table 3 should be moved to section 2.2.2.

It was made.

  1. There are two errors in the numbering of the references. The numbers 53 and 54 are repeated for the related references.

 It was corrected

  1. Authors must indicate clearly observed differences in the wavenumbers of peaks in the FT-IR spectra (Figure 4) with the bar line and still the quality of the figure needs to be improved. For example, the authors can simply use the horizontal legend, or delete the legends and insert the sample codes on each curve.

It was made.

Author Response File: Author Response.docx

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