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Article
Peer-Review Record

Degradation Kinetics of Automotive Shredder Residue and Waste Automotive Glass for SiC Synthesis: An Energy-Efficient Approach

Crystals 2023, 13(8), 1183; https://doi.org/10.3390/cryst13081183
by Sepideh Hemati *, Smitirupa Biswal, Farshid Pahlevani, Sanjith Udayakumar and Veena Sahajwalla
Reviewer 1: Anonymous
Reviewer 2:
Crystals 2023, 13(8), 1183; https://doi.org/10.3390/cryst13081183
Submission received: 13 June 2023 / Revised: 10 July 2023 / Accepted: 21 July 2023 / Published: 29 July 2023

Round 1

Reviewer 1 Report

1) The experimental section is poorly formatted. It should be divided into subsections for clarity reasons.

2) The isothermal experimants should be described in more detail. Was the sample heated in furnace from ambient temperature or sample was put into already heated to desired temperature furnace? What was the purpose of blowdown, if carbon oxides are nessecary for silicon carbide formation? How the mass balance and extent of reaction were determined, if no silicon carbide content in obtained sample was reported?

3) What is the purpose of the mechanism section? How occurrence of these reactions is proven? Reaction rate of which one was determined later in article?

4) All obtained activation energy values couldn't be refferred to any chemical reactions, but more likely to physical processes like evaporation or diffusion. This should be better discussed. Also the Figure 5c indicates, that activation energy value obtained for 650-750 C stage should be negative.

5) As long as all G(x) functions should be equal to 0 at x=0, approximating it via y=a*x+b function makes no sense. It is better to use y=a*x function.

6) The origin of the data for 3.2.2 section is unclear. The reaction rate calculation procedure should be described. What reaction rate was used for Figure 9? Maximal or mean?

There are many instances of "Error! Reference source not found." occurred in text. The correct references should be put there instead.

The degree of transformation in equation 1 is denoted by alpha, while in Table 1 same characteristic is denoted by x. I suppose the one symbol should be used for same parameter.

The equations for G(x) in Table 1 are lacking superscripts, which makes equations almost unrecognizable.

The reaction rate constant in Table 1 is denoted by k(T), while in equation 2 - by K.

I strongly recommend to change all values for linearized equations from decimal notation to scientific one (e.g. 2.1E-4 instead of 0.0002).

The experimental points in Figure 9 should be denoted by points, while calculated values - by lines.

Discussion and conclusion should be expanded in order to reveal underlying mechanisms. Right now it primarily simply states experimental results without further description.

Author Response

Response:

We would like to express our sincere appreciation for the time and effort you have dedicated to reviewing our paper. Your thoughtful and constructive comments have been immensely valuable to us, and we are delighted to see your interest in our research.

We have carefully considered each of your comments and suggestions and made corresponding revisions to address them. Below, we provide a detailed explanation and response to each of your points.

Once again, we sincerely thank you for your valuable input and for recognising the importance of our study. Your insights have undoubtedly contributed to the refinement of our work. We are grateful for your time and expertise, which have been instrumental in shaping the final version of our paper.

 

  • The experimental section is poorly formatted. It should be divided into subsections for clarity reasons.

 

Response:

  • The authors appreciate this practical comment by the reviewer. The Experimental section has been subdivided into three sections for more clarity, as suggested by the reviewer as follows:
  • Materials
  • Sample preparation
  • Characterisation
  • Kinetic study

 

  • The isothermal experimants should be described in more detail. Was the sample heated in furnace from ambient temperature or sample was put into already heated to desired temperature furnace? What was the purpose of blowdown, if carbon oxides are nessecary for silicon carbide formation? How the mass balance and extent of reaction were determined, if no silicon carbide content in obtained sample was reported?

 

Response:

  • The authors acknowledge and appreciate the valuable feedback provided by the reviewer. Their insights and suggestions have been carefully considered and incorporated into the revised version of the manuscript.
  • The extent of conversion was calculated using the data from off-gas analysis (Fig.S1 in supplementary file) through the carbon mass balance approach.

 

  • What is the purpose of the mechanism section? How occurrence of these reactions is proven? Reaction rate of which one was determined later in article?

Response:

  • The authors acknowledge and greatly appreciate the valuable comment provided by the reviewer. The reviewer's insights and suggestions have been thoroughly considered and implemented in the revised version of the manuscript.

 

  • Based on the literature, the formation mechanism of SiC production has been described in detail. Various mechanisms have been proposed to explain the formation of SiC from SiO2 and C reactions at high temperatures. The reaction kinetics is studied to understand the detailed mechanism of SiC synthesis. The reaction rate described in this part is for the synthesis of SiC from Mixed ASR and waste glass in the higher temperature range of 1300°C, 1400°C and 1500°C.
  • All obtained activation energy values couldn't be referred to any chemical reactions, but more likely to physical processes like evaporation or diffusion. This should be better discussed. Also the Figure 5c indicates, that activation energy value obtained for 650-750 C stage should be negative.

 

Response:

  • The authors would like to express their sincere acknowledgement and gratitude to the reviewer for providing a valuable comment. We greatly appreciate the reviewer's insights and suggestions, as they have been carefully considered and implemented in the revised version of the manuscript.

 

  • As long as all G(x) functions should be equal to 0 at x=0, approximating it via y=a*x+b function makes no sense. It is better to use y=a*x function.

 

Response:

 

  • The authors appreciate this practical comment by the reviewer. As recommended by the reviewer, all the G(x) functions in Figures 6 to 8 and Table 4 have been updated according to the y=a*x function.

 

  • The origin of the data for 3.2.2 section is unclear. The reaction rate calculation procedure should be described. What reaction rate was used for Figure 9? Maximal or mean?

 

Response:

  • We would like to express our appreciation for the valuable comment provided by the reviewer. The extent of conversion was calculated using the data from off-gas analysis (Fig.S1 in supplementary file) through the carbon mass balance approach. The reaction rate used is the mean value.

 

Comments on the Quality of English Language

  • There are many instances of "Error! Reference source not found." occurred in text. The correct references should be put there instead.

 

Response:

  • The authors thank the reviewer for this detailed comment. The mentioned sentence has been revised as suggested by the reviewer.

 

  • The degree of transformation in equation 1 is denoted by alpha, while in Table 1 same characteristic is denoted by x. I suppose the one symbol should be used for same parameter.

 

Response:

  • The authors appreciate the reviewer for this comment. As recommended by the reviewer, the degree of transformation in equation 1 is now denoted by x consistently, matching the notation used in Table 1.

 

  • The equations for G(x) in Table 1 are lacking superscripts, which makes equations almost unrecognisable.

 

Response:

  • The authors thank the reviewer for this useful comment. Table 1 has been updated in the manuscript to address the reviewer's comment.

 

  • The reaction rate constant in Table 1 is denoted by k(T), while in equation 2 - by K.

 

Response:

  • The authors very much appreciate the reviewer for this comment. The reaction rate constant in Equation (2) is now denoted by k(T) to be consistent with Table 1.

 

  • I strongly recommend to change all values for linearised equations from decimal notation to scientific one (e.g. 2.1E-4 instead of 0.0002).

 

Response:

  • The authors thank the reviewer for this comment. All numbers in this manuscript have been updated to scientific format as recommended by the reviewer.

 

  • The experimental points in Figure 9 should be denoted by points, while calculated values - by lines.

 

Response:

  • The authors appreciate the reviewer for their detailed comments. As recommended by the reviewer, Figure 9 has been updated in the manuscript to address their feedback.

 

  • Discussion and conclusion should be expanded in order to reveal underlying mechanisms. Right now it primarily simply states experimental results without further description.

 

Response:

  • The authors sincerely thank the reviewer for their valuable comments. We appreciate their insightful suggestion, and we have made the necessary revisions to the manuscript by expanding the mentioned sentence, as recommended by the reviewer.

 

Author Response File: Author Response.docx

Reviewer 2 Report

I reviewed your manuscript “

 Degradation Kinetics of Automotive Shredder Residue (ASR)  and Automotive Waste Glass for the In-situ Production of SiC  Nanoparticles” very judiciously. The work carried out in the manuscript is very interesting and seems scientifically logical. The authors have added good technical value and knowledge to synthesize SiC from novel method. However, there are numerous inaccuracies in this work and before publication, it needs to restructure the research manuscript properly and diligently as the current presentation is not acceptable. Therefore, I would like to recommend this article for "Major Revision".

1.    The title is not interesting. It should be meaningful and attractive. The author should clearly mentioned the removing agent.

2.    Arrange the keywords in alphabet order

3.    The author should report the latest and recent knowledge in introduction section.

4.     The authors should add the schematic diagram to show the mechanism of formation of SiC. See Journal of Materials Science: Materials in Electronics 32(7104):1-14 for this purpose.

5.    Table 1 format is not according to journal guidelines. Equation in all manuscript are also need to change according to MDPI guidelines

6.    In XRD section author claimed the SiC formation at 1300 and 1500 C but not give any reference of JCPdS card no. the author should also show the hkl values in the XRD figure. ·: SiC, ¨: SiO2,  :Ca(SiO3)  are always insight the figure.

7.    We cannot rely only on the XRD and EPMA for successful synthesize of the SiC. The author should provide more characterization like SEM, TEM, EDX and EDX mapping

8.    Formation mechanism should be included in the experimental section.

9.    Rearrange the fig 5 and Fig 7 according to MDPI guidelines.

10. Read the manuscript diligently and remove all the typographical, font style and font size mistakes

Author Response

"Degradation Kinetics of Automotive Shredder Residue (ASR)  and Automotive Waste Glass for the In-situ Production of SiC  Nanoparticles" very judiciously. The work carried out in the manuscript is very interesting and seems scientifically logical. The authors have added good technical value and knowledge to synthesise SiC from novel method. However, there are numerous inaccuracies in this work and before publication, it needs to restructure the research manuscript properly and diligently as the current presentation is not acceptable. Therefore, I would like to recommend this article for "Major Revision".

Response:

We would like to express our sincere appreciation for taking the time to carefully review our paper. Your insightful comments and constructive feedback have been invaluable to us. We are delighted to see your interest in our research and are grateful for your effort in providing thoughtful comments.

We have thoroughly considered your comments and provided a detailed explanation and response to each one below.

Once again, we would like to extend our gratitude for your valuable feedback. Your expertise and suggestions have greatly contributed to the improvement of our paper. We believe that your comments have enhanced our research's overall quality and clarity.

  1. The title is not interesting. It should be meaningful and attractive. The author should clearly mentioned the removing agent.

Response:

  • The authors thank the reviewer for this useful comment. To address the reviewer's comment, the author revised the title of the manuscript.

 

 

  1. Arrange the keywords in alphabet order

Response:

  • The authors appreciate the reviewer for this detailed comment. As recommended by the reviewer, the keywords have been rearranged alphabetically.

 

 

  1. The author should report the latest and recent knowledge in introduction section.

Response:

  • Thank you for your valuable comment. We appreciate your suggestion and understand the importance of providing up-to-date information in research articles. In response to your comment, we have thoroughly revised the manuscript to address this concern. We have conducted an extensive literature review to identify any recent developments, studies, or findings that are relevant to our research topic. We have updated the introduction section accordingly, ensuring that the latest and most pertinent information is included.

 

 

  1. The authors should add the schematic diagram to show the mechanism of formation of SiC. See Journal of Materials Science: Materials in Electronics32(7104):1-14 for this purpose.

Response:

  • The authors appreciate the reviewer for this comment. As recommended by the reviewer, the schematic diagram of the formation mechanism of SiC has been added in the manuscript.

 

  1. Table 1 format is not according to journal guidelines. Equation in all manuscript are also need to change according to MDPI guidelines

Response:

  • The authors thank the reviewer for this detailed comment. Table 1 has been updated according to MDPI guidelines.

 

  1. In XRD section author claimed the SiC formation at 1300 and 1500 C but not give any reference of JCPdS card no. the author should also show the hkl values in the XRD figure. ·: SiC, ¨: SiO2, :Ca(SiO3) are always insight the figure.

Response:

  • The authors would like to express their sincere gratitude to the reviewer for their valuable feedback on the manuscript. The authors have carefully considered the reviewer's comments and made appropriate revisions to address the raised points.

 

 

  1. We cannot rely only on the XRD and EPMA for successful synthesise of the SiC. The author should provide more characterisation like SEM, TEM, EDX and EDX mapping

Response:

  • We appreciate the reviewer's suggestion to include additional characterisation techniques. While we acknowledge the importance of these techniques in providing more comprehensive insights into the synthesised SiC material, the primary focus of our paper was on the kinetic aspects of the synthesis process. XRD was chosen as the main characterisation technique due to its effectiveness in demonstrating the formation of SiC and providing crystallographic information. We also want to mention that we chose EPMA over SEM-EDS to get relatively reliable quantification data at higher magnification using suitable standards and quantification method.

 

  1. Formation mechanism should be included in the experimental section.

Response:

  • The authors appreciate your suggestion regarding the inclusion of the formation mechanism in the experimental section. We have revised the manuscript accordingly, and the formation mechanism is now included in the experimental section as per your suggestion.

 

 

  1. Rearrange the fig 5 and Fig 7 according to MDPI guidelines.

Response:

  • The authors thank the reviewer for this detailed comment. We have cross-checked Figures 5 and 7 and all the other images and tables in our manuscript, ensuring they align with the prescribed MDPI guidelines.

 

  1. Read the manuscript diligently and remove all the typographical, font style and font size mistakes.

Response:

  • The authors sincerely appreciate the time and effort spent by the reviewer. The authors confirmed that the manuscript has been carefully reviewed, and diligently proofread it, addressing all typographical errors and inconsistencies in font style and size. To ensure the highest level of accuracy and readability, we have also engaged a native English speaker to review the manuscript.

 

 

 

 

Author Response File: Author Response.docx

Round 2

Reviewer 2 Report

Dear author, i am satisfied by the response submitted by you but still keywords are not in alphabet order.

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