Additive Manufacturing of Ti₃AlC₂/TiC and Ti₃AlC₂/SiC Ceramics Using the Fused Granules Fabrication Technique

Round 1

Reviewer 1 Report

Comments and Suggestions for Authors

The authors provided a work on the 3D printing of ceramics. Two samples were selected, TiC:TAC and SiC:TAC composites. Overall, this manuscript was prepared well and substantially presented some interesting results for readers. Several minor revisions are listed below  for the authors to take a further step to improve the article. 

First, some grammar errors need be corrected, such as page 4 line 159, the reference No. is missing. 

Second, I'm interesting in the structure evolution of the samples in each step, so please provide the morphological images of the samples after being printed, debonding, sintering and bend-fractured. 

Third, when talking about the setting of printing parameters, e.g., Slicered calibration model, extra refereces can be cited, such as Additive Manufacturing, 2021, 47, 102267. https://doi.org/10.1016/j.addma.2021.102267. Similar references can be cited to comfirm the idea which the authors discussed.

Comments on the Quality of English Language

The English writing is good. 

Author Response

Dear Reviewer! On behalf of the of the article, we thank you for your work and the time you have devoted to our article. Your comments have undoubtedly let us to improve the manuscript. We have tried to take all your comments into account. You can find our responses below.

The authors provided a work on the 3D printing of ceramics. Two samples were selected, TiC:TAC and SiC:TAC composites. Overall, this manuscript was prepared well and substantially presented some interesting results for readers. Several minor revisions are listed below  for the authors to take a further step to improve the article. 

First, some grammar errors need be corrected, such as page 4 line 159, the reference No. is missing. 

Thank you for your comment. The mistake is corrected.

Second, I'm interesting in the structure evolution of the samples in each step, so please provide the morphological images of the samples after being printed, debonding, sintering and bend-fractured.

Thank you for your comment. Fig. 1 provides the structure of the green samples. Fig. 6 and 8 provides the structure of the sintered samples. Only the structure of the brown samples is not providing since after debinding the samples become brittle. In general, the structure is nearly the same as for green samples, but more porous since the polymer binder was removed during the debinding stage.

Third, when talking about the setting of printing parameters, e.g., Slicered calibration model, extra refereces can be cited, such as Additive Manufacturing, 2021, 47, 102267. https://doi.org/10.1016/j.addma.2021.102267. Similar references can be cited to comfirm the idea which the authors discussed.

Thank you for your comment. The mentioned article is really interesting and was added to the reference list.

Reviewer 2 Report

Comments and Suggestions for Authors

I've reviewed the paper titled "Additive Manufacturing of Ti3AlC2/TiC and Ti3AlC2/SiC Ceramics Using Fused Granules Fabrication Technique." It dives into how ceramic composites are made using additive manufacturing. This study is pretty insightful, especially about the fused granules fabrication method and using it to create ceramic composites with different properties. Though, there are a few points that could use some work to make the paper even better and ready for publication.

1. The intro's good but could really shine by diving deeper into why the FGF technique's better or different than other methods.  

2. In Section 2.1 about Feedstock Preparation, we need more on why specific polymer binders and their ratios were picked. How do these choices affect the end product?

3. The Fabrication part (Section 2.2) lacks some key details on optimizing the FGF process. Stuff like layer thickness, nozzle temperature – these are important and should be mentioned.

4. The Characterization part (Section 3.3) could do with more stats analysis on the mechanical testing results. It's about making sure the data's solid and the conclusions are trustworthy.

5. Noticed some figures aren't talked about much or at all in the text. Every figure needs to be clearly discussed and linked back to what's being concluded.

6. The conclusions are kinda broad. It'd be great if they tied back more directly to the findings talked about in the paper. Like, each big conclusion should have a call back to the results that support it.

7. Some references seem slightly off or irrelevant to what's being said. It's important that all citations back up the claims and are current.

This paper has much potential to add something valuable to the materials science and additive manufacturing fields. With a bit of tweaking, especially on the method details, data analysis, and discussion depth, it could really make a strong case for the production and properties of Ti3AlC2/TiC and Ti3AlC2/SiC composites using the FGF technique.

Comments on the Quality of English Language

The manuscript is generally well-written, with a few instances of awkward phrasing and grammatical errors that slightly hinder the clarity of the text. To enhance the readability and professionalism of the paper, I recommend the following specific improvements:

There are occasional grammatical mistakes and awkward constructions that need to be revised. For example, the use of tense is sometimes inconsistent, and there are missing articles before certain nouns.

Ensure that technical terms and jargon are used consistently throughout the paper. There are a few instances where terms are introduced without sufficient explanation or are used interchangeably without clarification.

Some sentences are overly complex and could be simplified for better understanding. Breaking down long sentences and using more straightforward language would help in conveying complex information more clearly.

Some sections contain dense technical content that could be better explained. Consider adding more transitional phrases to guide the reader through the discussion, especially when introducing new topics or complex data.

Pay attention to the use of commas and semicolons for proper separation of clauses and to enhance the flow of information. Also, ensure that all figures and tables are properly formatted and clearly referenced in the text.

Ensure consistency in the spelling of technical terms, especially those that can have multiple spellings (e.g., "fiber" vs. "fibre"). Decide on one spelling and stick to it throughout the document.

Author Response

Dear Reviewer! On behalf of the of the article, we thank you for your work and the time you have devoted to our article. Your comments have undoubtedly let us to improve the manuscript. We have tried to take all your comments into account. You can find our responses below.

1. The intro's good but could really shine by diving deeper into why the FGF technique's better or different than other methods.

Thank you for your comment. The introduction section was enhanced and more information about FGF was added.

2. In Section 2.1 about Feedstock Preparation, we need more on why specific polymer binders and their ratios were picked. How do these choices affect the end product?

Thank you for your comment. Details on binder ratios was added. This choice is explained by technological conditions – from the microstructure point of view we need as less polymer as possible to achieve the maximum density of the samples, but from flowability point of view we need as more polymer as possible to achieve maximum melt flow index of the feedstock. The ratio used is an optimum ratio to achieve high density of the samples with good flowability. More data on feedstock investigation is in our previous paper (https://doi.org/10.3390/coatings13061013).

3. The Fabrication part (Section 2.2) lacks some key details on optimizing the FGF process. Stuff like layer thickness, nozzle temperature – these are important and should be mentioned.

Thank you for your comment. The mentioned parameters were listed in lines 189-191 in the original manuscript, now it was added in Section 2.2.

4. The Characterization part (Section 3.3) could do with more stats analysis on the mechanical testing results. It's about making sure the data's solid and the conclusions are trustworthy.

Thank you for your comment. The paper presents the final data on the results of mechanical tests. 5-7 samples of each composition were tested. Based on the data obtained, the average value and standard deviation were calculated. The statistically obtained data are sufficient to confirm the correctness of the tests.

5. Noticed some figures aren't talked about much or at all in the text. Every figure needs to be clearly discussed and linked back to what's being concluded.

Thank you for your comment. We additionally checked and fixed the indicated problem.

6. The conclusions are kinda broad. It'd be great if they tied back more directly to the findings talked about in the paper. Like, each big conclusion should have a call back to the results that support it.

Thank you for your comment. The conclusion section was rewritten.

7. Some references seem slightly off or irrelevant to what's being said. It's important that all citations back up the claims and are current.

Thank you for your comment. We revised all references and make some changes. However, on our opinion all references are relevant to the investigation by some places in text and title of the cited paper may be confusing.

Reviewer 3 Report

Comments and Suggestions for Authors

Paper ‘Additive Manufacturing of Ti3AlC2/TiC and Ti3AlC2/SiC Ceramics Using Fused Granules Fabrication Technique’ examines the effect of ceramic content on the densification and mechanical properties of SiC-Ti3AlC2 and TiC-Ti3AlC2 composites produced by additive manufacturing. Some questions should be added to improve the quality of the manuscript.

1.     The logic of the introduction is not sound enough. The introduction should comprehensively analyze the limitations of ceramic composite additive manufacturing and then introduce the research objectives of this paper.

2.     The section 3.1 Parameters of Additive Manufacturing looks like a lab report. How do the parameters affect the forming quality and what are the internal mechanisms of how to select them that should be discussed.

3.     In section 3.3 Structure, Phase Composition and Mechanical Properties, some phase, such as Ti2AlC phase, Ti3AlC2, Sn phase, was observed in XRD spectra. This XRD measurement is not sufficient to define the presence of these phases and should be further determined in conjunction with other elemental analyses, such as TEM, EDS, etc.

Author Response

Dear Reviewer! On behalf of the of the article, we thank you for your work and the time you have devoted to our article. Your comments have undoubtedly let us to improve the manuscript. We have tried to take all your comments into account. You can find our responses below.

1. The logic of the introduction is not sound enough. The introduction should comprehensively analyze the limitations of ceramic composite additive manufacturing and then introduce the research objectives of this paper.

Thank you for your comment. The introduction was rewritten.

2. The section 3.1 Parameters of Additive Manufacturing looks like a lab report. How do the parameters affect the forming quality and what are the internal mechanisms of how to select them that should be discussed.

Thank you for your comment. Our investigation is mainly related with technological parameters (this is one of the reasons why we choose JMMP) so it may look like lab report. However, we improved this section according to your comment.

3. In section 3.3 Structure, Phase Composition and Mechanical Properties, some phase, such as Ti2AlC phase, Ti3AlC2, Sn phase, was observed in XRD spectra. This XRD measurement is not sufficient to define the presence of these phases and should be further determined in conjunction with other elemental analyses, such as TEM, EDS, etc.

Thank you for your comment. Of course, XRD alone is not enough to determine all phases. However, we used an integrated approach to establish the specified phases. We relied on literature data and previously obtained experience in working with the MAX phase, including the study of its decomposition (https://doi.org/10.3390/coatings13061013 https://doi.org/10.3390/ma16041537 https://doi.org/10.3390/coatings12121928 https://doi.org/10.1134/S2075113322030212 https://doi.org/10.1080/17436753.2022.2121460). In the above-mentioned works, the areas corresponding to the required phases were localized using SEM. Since the main objective of the present work was to determine the optimal parameters for obtaining samples, the emphasis was not placed on the materials science part.

Reviewer 4 Report

Comments and Suggestions for Authors

1、it is recommended to add the fused granules fabrication (FGF) method, spark plasma sintering (SPS) printing equipment and print sample pictures.

2、The format of the manuscript needs to be carefully revised, such as section 3.1, paragraph 4 “[]” is not standardized.

3、Should be unified picture title format.

4、Why is there no mark in the text of the manuscript in Figure 5?

Comments on the Quality of English Language

Minor editing of English language required

Author Response

Dear Reviewer! On behalf of the of the article, we thank you for your work and the time you have devoted to our article. Your comments have undoubtedly let us to improve the manuscript. We have tried to take all your comments into account. You can find our responses below.

1、it is recommended to add the fused granules fabrication (FGF) method, spark plasma sintering (SPS) printing equipment and print sample pictures.

Thank you for your comment. The article provides a complete list of the equipment used. Unfortunately, the article already has many drawings and we did not add a new one with the equipment. The appearance of the printed sample is shown in Figure 3. The appearance of the SPS samples - tablets, is also not shown in the article for reasons of space saving. The most interesting sample is obtained by additive technologies, since it is most likely to be destroyed during the printing process, which did not happen in our case.

2、The format of the manuscript needs to be carefully revised, such as section 3.1, paragraph 4 “[]” is not standardized.

Thank you for your comment. This mistake was corrected.

3、Should be unified picture title format.

Thank you for your comment. The picture title format was unified.

4、Why is there no mark in the text of the manuscript in Figure 5?

The reference to all figures was checked throughout the text and all missed references was added.

Reviewer 5 Report

Comments and Suggestions for Authors

This paper has presented” Additive manufacturing of Ti₃AlC₂/Tic and Ti₃AlC₂/Sic ceramics using fused granules fabrication technique”, there are some issues that need to be addressed before the manuscript can be accepted by the journal.

1)      There are several grammatical errors throughout the text, including punctuation issues, sentence fragments, and awkward phrasing. It is essential to ensure that the text is grammatically correct to maintain clarity and professionalism.

2)      The abstract is too short and lacks the main achievements of this study. Please modify the abstract properly and add the most important achievements.

3)      Please provide a more comprehensive discussion about the properties of MAX phases for high-temperature applications. Below are some references to help with this issue.

-          Microstructure and mechanical properties of hot-pressed Ti–Co–Si compounds reinforced by intermetallic phases, Materials Characterization Volume 171, January 2021, 110816.

-          Effect of Ti3AlC2 MAX Phase on Structure and Properties of Resultant Ti3C2Tx MXene, ACS Appl. Nano Mater. 2019, 2, 6, 3368–3376. 

4)      Please provide more information in the Materials and Methods section about how the powders were mixed. What is high-energy ball milling or simple milling for mixing?

5)      In the following sentence, the reference is missing: 'The selection of the correct temperature was carried out at the feedstock development stage []'

 

6)      A more comprehensive comparison between the samples manufactured by Fused Granules Fabrication (FGF) method and Spark Plasma Sintering (SPS) in terms of mechanical properties is needed. Could we conduct a hardness test to facilitate this comparison?

Comments on the Quality of English Language

here are several grammatical errors throughout the text, including punctuation issues, sentence fragments, and awkward phrasing. It is essential to ensure that the text is grammatically correct to maintain clarity and professionalism

Author Response

Dear Reviewer! On behalf of the of the article, we thank you for your work and the time you have devoted to our article. Your comments have undoubtedly let us to improve the manuscript. We have tried to take all your comments into account. You can find our responses below.

1)      There are several grammatical errors throughout the text, including punctuation issues, sentence fragments, and awkward phrasing. It is essential to ensure that the text is grammatically correct to maintain clarity and professionalism.

Thank you for your comment. The manuscript was carefully revised.

2)      The abstract is too short and lacks the main achievements of this study. Please modify the abstract properly and add the most important achievements.

Thank you for your comment. The abstract was rewritten.

3)      Please provide a more comprehensive discussion about the properties of MAX phases for high-temperature applications. Below are some references to help with this issue.

-          Microstructure and mechanical properties of hot-pressed Ti–Co–Si compounds reinforced by intermetallic phases, Materials Characterization Volume 171, January 2021, 110816.

-          Effect of Ti3AlC2 MAX Phase on Structure and Properties of Resultant Ti3C2Tx MXene, ACS Appl. Nano Mater. 2019, 2, 6, 3368–3376. 

Thank you for your suggestion. The article “Effect of Ti3AlC2 …” was added to the reference list.

4)      Please provide more information in the Materials and Methods section about how the powders were mixed. What is high-energy ball milling or simple milling for mixing?

Thank you for your comment. We used simple dry mixing, the description was added to the Materials and Methods section.

5)      In the following sentence, the reference is missing: 'The selection of the correct temperature was carried out at the feedstock development stage []'

 Thank you for your comment. The missing reference was added.

6)      A more comprehensive comparison between the samples manufactured by Fused Granules Fabrication (FGF) method and Spark Plasma Sintering (SPS) in terms of mechanical properties is needed. Could we conduct a hardness test to facilitate this comparison?

Thank you for your comment. The microhardness test was conducted, the results was added to the manuscript.

Round 2

Reviewer 2 Report

Comments and Suggestions for Authors

I am writing to convey my recommendations regarding the manuscript titled "Additive Manufacturing of Ti3AlC2/TiC and Ti3AlC2/SiC Ceramics Using Fused Granules Fabrication Technique," manuscript ID jmmp-3017110. Upon reviewing the revised version submitted for the second round of peer review, it is clear that the authors have diligently addressed the concerns and suggestions presented during the initial review process.

The comprehensive revisions and the quality of data presented have elevated the manuscript to meet the publication standards of the journal. The findings contribute valuable insights into the additive manufacturing processes for ceramic composites, which are of great relevance to ongoing research in advanced material sciences.

Therefore, I recommend the publication of this manuscript. The authors have presented a well-structured study with reliable data and sufficient discussion, which will undoubtedly provide a strong experimental foundation for the application and further development of these composite materials.