Microstructure and Mechanical Properties of Titanium–Equine Bone Biocomposites
Round 1
Reviewer 1 Report
Dear authors,
You did an interesting work but the presentation of it does not satisfy. My remarks are as follows:
P1 L16: Mark for Vickers hardness is HV, not Hv
Generally, in the Introduction section should be given the current state of the research field. Therefore, used references should be of newer dates than presented in this paper, especially since there is really a lot of new literature on this subject.
P1 L23-31: Namely, there are many attempts of adding the various elements (Nb, Zr, Ta, Sn) to titanium regarding the improvement of its properties, such as:
[7] YEMISCI, I., MUTLU, O., GULSOY, N., KUNAL, K., ATRE, S., GULSOY, H.O. Experimentation and analysis of powder injection molded Ti10Nb10Zr alloy: a promising candidate for electrochemical and bioemdical application, Journal of Materials Research and Technology. 2019, vol. 8, no. 6, pp. 5233-5245.
[8] SLOKAR, LJ, ŠTRKALJ, A., GLAVAŠ, Z. Synthesis of Ti-Zr alloy by powder metallurgy, Engineering Review. 2019, vol. 39, no. 1, pp. 115-123.
[9] WALLY, Z.J., VAN GRUNSVEN, W., CLAEYEESNS, F., GOODAL, R., REILLY, G.C. Porous titanium for dental implant applications, Metals. 2015, vol. 5, pp. 1902-1920.
P2 L44-46: should be included following references:
ARIFIN, A., BAKAR, A., MUHAMAD, N., SYARIF, J., RAMLI, M.I. Material processing of hydroxyapatite and titanium alloy (HA/Ti) composite as implant materials using powder metallurgy: A review, Materials and Design. 2014, vol. 55, pp. 165–175
LI, F., JIANF, X., SHAO, Z., ZHU, D., LUO, Z. Research Progress Regarding Interfacial Characteristics and the Strengthening Mechanisms of Titanium Alloy/Hydroxyapatite Composites. Materials. 2018, vol. 11, no. 8, pp. 1391
P2 L70 and 72: micron missing (µ)
P2 L69-73: in which ratio were starting powders (Ti6Al4V and EB) or please give the mass of each starting powder in a mill.
P2 L73: In which atmosphere milling was performed?
P2 L74: “…followed by a 40 min pause to avoid overheating.” It is not clear when was that pause? After 12h? When was then the end of milling?
P2 L75: Which atmosphere was in the steel bowl?
P2 L80: “…and maintained for 15 min at an applied pressure of 50 MPa...” In Abstract: “…
10 minutes under 50 MPa” Which time is a correct?
P2 L83: having ® have
P2 L85: What does it mean: “The power morphologies of the starting powders...”?
P2 L88-89, P3 L107-108, P5 L120-122,125 and so on: some symbols are missing
P2 L95-96: there are repeating for 2 times “were performed”
P2 L98: How many measurements of nano-indentation were performed on each specimen? Please describe Vickers hardness measurements that were conducted.
P3 L113: How it was checked whether there was or was no contamination of powders by steel from mill?
P4: SEM figures (a) and (b) should be given at the same magnification. Also (d) should be given at the same magnifications as (f) and (h) to be comparable
P5: Caption of Figure 1 is a little bit confusing regarding a, b, c… please, give it more clearly. Further, Figure 1 (i) should be a Figure 2 since it is not a SEM image
P5 L124-125: “As the reference, defects such as pores and voids were not found in the Ti6Al4V sintered 124 -Ti were 12.6 %.” Please explain how it is possible that in the sintered samples there are no pores.
P5: Figure 2(e) should be another figure. Further, what is the accuracy of the EDS method? I know that software gives results with 2 decimals, but the method is only semi-quantitative and therefore they have no sense. Also, which is a reliable limit of detectability of used EDS detector? Namely, fractions of P, Ca, O should be listed with the caution. How did fractions determined? By measuring in how many points/spots? Are in the table a mean values listed? How much is the deviation?
P6 L135-136: “The significance in f is closely related to elastic modulus, which is an important factor as a biomedical material to attain low elastic modulus” please give a clearer sentence.
P7: XRD profiles for EB shows some unidentified peaks. Why? Further, how can you be sure that in sintered T-0.5EB and T-0.05EB is beta phase present, when you showed that beta peak exists at only one angle? How can you explain that in sintered T-5EB beta phase does not exists?
P8 L185-187: please specify the proper process conditions that will result in suitable properties (elastic modulus) for biomedical use.
P8: Figure 4a: can you explain why the increase in elastic modulus does not accompany the increase in hardness. Or, why is the modulus for T-0.5EB lower than modulus for T-0.05EB and T-5EB?
P9 L209-210: in conclusion, the most important obtained results should be emphasized and not the recommendations.
Conclusion should be improved after corrections made in main text.
Extensive editing of English language and style are required.
Author Response
Response to Reviewer 1 Comments
Dear authors,
You did an interesting work but the presentation of it does not satisfy. My remarks are as follows:
Comments 1: P1 L16: Mark for Vickers hardness is HV, not Hv
Authors response : Thank you for your comments, and we revised the unit as “HV” in the abstract.
Comments 2: Generally, in the Introduction section should be given the current state of the research field. Therefore, used references should be of newer dates than presented in this paper, especially since there is really a lot of new literature on this subject. P1 L23-31: Namely, there are many attempts of adding the various elements (Nb, Zr, Ta, Sn) to titanium regarding the improvement of its properties, such as:[7] YEMISCI, I., MUTLU, O., GULSOY, N., KUNAL, K., ATRE, S., GULSOY, H.O. Experimentation and analysis of powder injection molded Ti10Nb10Zr alloy: a promising candidate for electrochemical and bioemdical application, Journal of Materials Research and Technology.2019, vol. 8, no. 6, pp. 5233-5245.[8] SLOKAR, LJ, ŠTRKALJ, A., GLAVAŠ, Z. Synthesis of Ti-Zr alloy by powder metallurgy, Engineering Review. 2019, vol. 39, no. 1, pp. 115-123. [9] WALLY, Z.J., VAN GRUNSVEN, W., CLAEYEESNS, F., GOODAL, R., REILLY, G.C. Porous titanium for dental implant applications, Metals. 2015, vol. 5, pp. 1902-1920.
Authors response : Thank you for your comments, and we replaced the references as your advice.
[1] Z.J. Wally, W. Van Grunsven, F. Claeyssens, R. Goodall, G.C. Reilly, Metals 5, 1902 (2015).
[2] I. Yemisci, O. Mutlu, N. Gulsoy, K. Kunal, S. Atre, H.O. Gulsoy, Journal of Materials Research and Technology 8, 5233 (2019).
[3] L. Slokar, A. Štrkalj, Z. Glavaš, Engineering Review 39, 115 (2019).
Comments 3: P2 L44-46: should be included following references: ARIFIN, A., BAKAR, A., MUHAMAD, N., SYARIF, J., RAMLI, M.I. Material processing of hydroxyapatite and titanium alloy (HA/Ti) composite as implant materials using powder metallurgy: A review, Materials and Design. 2014, vol. 55, pp. 165–175 LI, F., JIANF, X., SHAO, Z., ZHU, D., LUO, Z. Research Progress Regarding Interfacial Characteristics and the Strengthening Mechanisms of Titanium Alloy/Hydroxyapatite Composites. Materials. 2018, vol. 11, no. 8, pp. 1391
Authors response : Thank you for your comments, and we added the references as your advice.
[19] A. Arifin, A.B. Sulong, N. Muhamad, J. Syarif, M.I. Ramli, Mater. Design. 55, 165 (2014).
[21] F. Li, X. Jiang, Z. Shao, D. Zhu, Z. Luo, Materials 11, 1391 (2018).
Comments 4: P2 L70 and 72: micron missing (µ)
Authors response : Thank you for your comments, we did put the right unit, however during the transferring to a pdf file, it was missing. We will check before the publication.
Comments 5: P2 L69-73: in which ratio were starting powders (Ti6Al4V and EB) or please give the mass of each starting powder in a mill.
Authors response : As your comments, we put the information as shown below in the manuscript.
“The Ti6Al4V-EB composite powders of 50 g were…”
Comments 6: P2 L73: In which atmosphere milling was performed? P2 L74: “…followed by a 40 min pause to avoid overheating.” It is not clear when was that pause? After 12h? When was then the end of milling? P2 L75: Which atmosphere was in the steel bowl?
Authors response : As your comments, we put the information as shown below in the manuscript.
“…a rotational speed of 200 RPM for 12 h, followed by a 40 min pause after every 20 min of milling to avoid overheating under air atmosphere.”
Comments 7: P2 L80: “…and maintained for 15 min at an applied pressure of 50 MPa...” In Abstract: “… 10 minutes under 50 MPa” Which time is a correct?
Authors response : We apologize for the confusion, and we revised the as “ …15 minutes” in the abstract.
Comments 8: P2 L83: having ® have
P2 L85: What does it mean: “The power morphologies of the starting powders...”?
P2 L88-89, P3 L107-108, P5 L120-122,125 and so on: some symbols are missing
P2 L95-96: there are repeating for 2 times “were performed”
Authors response : We apologize for confusion, and we have revised all grammatical error very carefully, and the changes are highlighted in red.
Comments 9: P2 L98: How many measurements of nano-indentation were performed on each specimen? Please describe Vickers hardness measurements that were conducted.
Authors response : We measured the nano-indentation more than 10 times for the data accuracy, and we put the information in the manuscript, as shown below.
”… indenter and measured more than 12 times per each specimen. … The Vickers hardness of the specimens was measured using a micro-Vickers hardness testing machine (Mitutoyo, HM200, Japan) with an indenter load of 300 N.”
Comments 10: P3 L113: How it was checked whether there was or was no contamination of powders by steel from mill?
Authors response : We checked all the powders through EDS analysis during the SEM observation, however the Fe element from the steel balls cannot find. Moreover, not only broken steel balls did not find after planetary ball-milling, but also input and output ratio of the powders were below 90%, therefore the contamination from the Fe element within the steel balls has nearly possible.
Comments 11: P4: SEM figures (a) and (b) should be given at the same magnification. Also (d) should be given at the same magnifications as (f) and (h) to be comparable
Authors response : We apologized the error of scale bar and revised the SEM image in Fig. 1(d) as shown below.
Comments 12: P5: Caption of Figure 1 is a little bit confusing regarding a, b, c… please, give it more clearly. Further, Figure 1 (i) should be a Figure 2 since it is not a SEM image.
Authors response : We tried to change as your comments, however, the elemental results in Fig. 1(i) come from the exact image of Fig.1, therefore, we decide to keep this figure caption for readability.
Comments 13: P5 L124-125: “As the reference, defects such as pores and voids were not found in the Ti6Al4V sintered 124 -Ti were 12.6 %.” Please explain how it is possible that in the sintered samples there are no pores.
Authors response : We examined the bulk samples as shown below, large pore excluding Ti6Al4V-5EB composites. Therefore we measured the density and porosity, all the sintered samples having a porosity below 2% and relative density above 99%. The revised sentences are as shown below.
In page 6: “As the reference, defects such as pores and voids were not significantly found.... The sintered composites having a porosity below 1% and relative density above 99% on average, excluding Ti6Al4V-5EB composites.”
|
Porosity:0.06% 0.17% 8.2% |
Comments 14: P5: Figure 2(e) should be another figure. Further, what is the accuracy of the EDS method? I know that software gives results with 2 decimals, but the method is only semi-quantitative and therefore they have no sense. Also, which is a reliable limit of detectability of used EDS detector? Namely, fractions of P, Ca, O should be listed with the caution. How did fractions determined? By measuring in how many points/spots? Are in the table a mean values listed? How much is the deviation?
Authors response : We changed Fig. 2(e) to Table 1, and we know well detectability of EDS detector. Therefore, we did focus only relative comparison between the composites as a function of EB contents rather than the numerical contents of each elemental composition.
“Also, the chemical compositions for each phase from EDS analysis have shown in Table 1”
Fig. 2 SEM images and EDS analysis of ball-milled Ti6Al4V-EB composites under different weight fraction of the EB; (a) T-0.05Ed; (b) T-0.5EB and (c) T-5EB.
Comments 15: P6 L135-136: “The significance in f is closely related to elastic modulus, which is an important factor as a biomedical material to attain low elastic modulus” please give a clearer sentence.
Authors response : We revised to provide clear sentence and revised as shown below.
“The significance in fβ is closely related to elastic modulus, which is an important factor as a biomedical material to attain low elastic modulus, because, beta phase has a low elastic modulus than alpha phase. [32-34]. Stress shielding effect can occur according to high elastic modulus, therefore, a decrease in elastic modulus is important for apply biomedical implants [34-37].”
Comments 16: P7: XRD profiles for EB shows some unidentified peaks. Why? Further, how can you be sure that in sintered T-0.5EB and T-0.05EB is beta phase present, when you showed that beta peak exists at only one angle? How can you explain that in sintered T-5EB beta phase does not exists?
Authors response : We revised the XRD plots in Fig. 3 as shown below.
Comments 17: P8 L185-187: please specify the proper process conditions that will result in suitable properties (elastic modulus) for biomedical use.
Authors response : We revised the sentence as shown below.
“…this result showed that the proper selection of process conditions for the fabrication of Ti6Al4V matrix composites could have high strength and suitable elastic modulus for use as biomedical implants. For instance, when the composites sintered above 1200 oC, hydroxyapatite can phase transformed to meta-stable phase such as tricacium phosphate, which may lead to biodegradation in the human body [40] .”
Comments 18: P8: Figure 4a: can you explain why the increase in elastic modulus does not accompany the increase in hardness. Or, why is the modulus for T-0.5EB lower than modulus for T-0.05EB and T-5EB?
Authors response : As we responded the comments #13, the mechanical properties are strongly related to the density. For the SPSed composites, the porosity of the Ti6Al4V-0.5EB composites (0.17%) is higher than Ti6Al4V-0.05EB composites (0.06%). Therefore, the elastic modulus also decreased for the Ti6Al4V-0.5EB composites compare to Ti6Al4V-0.05EB composites.
In Page 8: “Further, the elastic modulus of the SPSed samples are affected by the density, for the Ti6Al4V-0.5EB composites, it showed the lowest elastic modulus due to having a relatively low density of 95%.”
Comments 19: P9 L209-210: in conclusion, the most important obtained results should be emphasized and not the recommendations. Conclusion should be improved after corrections made in main text. Extensive editing of English language and style are required.
Authors response : We removed misleading sentences as the reviewer’s comment. And, we proofread all manuscript, and figure and table captions.
All contents mentioned in this rebuttal are also addressed in the manuscript. The changes in the manuscript are highlighted in red.
With best regards,
Se-Eun Shin (Corresponding author)
Assistant Professor
Department of Materials Science and Metallurgical Engineering, Sunchon National University, Korea
E-mail: [email protected], TEL:+82-61-750-3553, FAX: +82-61-750-3550
Author Response File: 
Author Response.pdf
Reviewer 2 Report
Biomedical implants are coated with a layer of hydroxyapatite to improve its engraftment in living matter. However, a detachment of hydroxyapatite from a metallic substrate occurs. The authors predict an improvement in the quality of engraftment by changing the technology of manufacturing the implant. In particular, it is possible to manufacture an implant using a combination ball milling and spark plasma sintering of hydroxyapatite powders and metal implant. The authors indicate the purpose of the article to develop the fabrication process using powder metallurgy and overcome the peeling of the hydroxyapatite from the chosen Ti6Al4V alloy as implant material. Powders were mixed and sintered.
Their structure and properties were also investigated. There are no data on overcoming pilling in the article. The article contains inaccuracies.
Lines 110, 111 of text. Accordingly, EB powders were not observed on the Ti6Al4V powder surface in all composite powders….
Then it should be recognized that the hydroxyapatite particles dissolved during ball milling. Only a study of the elemental composition cannot be evidence of their absence.
Lines 120, 121. …..the face-centered cubic (FCC) and the body-centered cubic (BCC) phases….
Phases with hexagonal close-packed and body-centered lattices are present in titanium alloys.
Lines 124,125. Correctly use the term volume fraction of phase rather than amount.
Line 133. The authors inform that…..and Ti were found to be approximately 3:2 and 3:4, respectively (in Fig. 2e).
Why is this information given and what does it mean? The authors do not discuss.
Line 134. The V concentration in the Ti matrix increased according to the Ti phase transformation.
However, there is no data on the definition and change of this characteristic.
Figure 3 b, there is no synthesized sample with the highest content of EB lines corresponding to the beta phase in the X-ray diffraction pattern.
Meanwhile, the beta phase is present in the microstructure. This difference should be explained.
Line 175. …particle strengthening effects on the hardness increment.
No evidence of this result. This result can only be expressed as an assumption.
Line 179. However, it depends on the fraction of b-Ti among the composites.
An error should be given in determining the volume fraction of the beta phase.
Line 204. The hardness of the Ti6Al4V-EB composites increased as the EB contents increase owing to uniformly distribution of EB in the Ti6Al4V matrix.
No evidence of uniformly distribution.
Line 205. The composites SPSed at 1000 oC, which is beta-phase transformation temperature, showed stable elastic modulus.
The research results showed that the elastic modulus varies markedly depending on the composition of the alloys. What stability modulus are the authors talking about?
Line 210. The authors suggest that additional heat treatment can decrease the elastic modulus.
What article results demonstrate this effect?
The article contains numerous errors showing poor English proficiency.
In sum, careful work is required, both with the results obtained and with the text of the article. The article is needed major revision.
Author Response
Response to Reviewer 2 Comments
Biomedical implants are coated with a layer of hydroxyapatite to improve its engraftment in living matter. However, a detachment of hydroxyapatite from a metallic substrate occurs. The authors predict an improvement in the quality of engraftment by changing the technology of manufacturing the implant. In particular, it is possible to manufacture an implant using a combination ball milling and spark plasma sintering of hydroxyapatite powders and metal implant. The authors indicate the purpose of the article to develop the fabrication process using powder metallurgy and overcome the peeling of the hydroxyapatite from the chosen Ti6Al4V alloy as implant material. Powders were mixed and sintered. Their structure and properties were also investigated. There are no data on overcoming pilling in the article. The article contains inaccuracies.
Comments 1 : Lines 110, 111 of text. Accordingly, EB powders were not observed on the Ti6Al4V powder surface in all composite powders…. Then it should be recognized that the hydroxyapatite particles dissolved during ball milling. Only a study of the elemental composition cannot be evidence of their absence.
Author’s response : As the reviewer’s comment, we added Figure 2 as shown below to reveal the hydroxyapatite particles as ball-milled Ti6Al4V-EB powders with EDS analysis.
Comments 2 : Lines 120, 121. …..the face-centered cubic (FCC) and the body-centered cubic (BCC) phases…. Phases with hexagonal close-packed and body-centered lattices are present in titanium alloys.
Authors response : We apologized for the confusion and revised the manuscript as shown below.
“…α-Ti with the hexagonal closed packed (HCP)”
Comments 3 : Lines 124,125. Correctly use the term volume fraction of phase rather than amount.
Authors response : We apologize for the confusion, the volume fraction has correct, therefore we revised the term in the manuscript as shown below.
“… a volume fraction of β-Ti phase (fβ) … ”
Comments 4 : Line 133. The authors inform that…..and Ti were found to be approximately 3:2 and 3:4, respectively (in Fig. 2e). Why is this information given and what does it mean? The authors do not discuss. Line 134. The V concentration in the Ti matrix increased according to the Ti phase transformation. However, there is no data on the definition and change of this characteristic.
Authors response : The existence of beta phase in the composites is important because it affects the elastic modulus. For beta phase, vanadium is a beta phase stabilizing element, the ratio of aluminum and vanadium 3:4 should be maintained in the beta phase. Therefore, we included this information, and for readability, we added the references in the manuscript to back up this information.
“…respectively (in Fig. 3e) [31].”
[31] S. Semiatin, S. Knisley, P. Fagin, D. Barker, F. Zhang, Metallurgical and Materials Transactions A 34, 2377 (2003).
Comments 5 : Figure 3 b, there is no synthesized sample with the highest content of EB lines corresponding to the beta phase in the X-ray diffraction pattern. Meanwhile, the beta phase is present in the microstructure. This difference should be explained.
Authors response : We put the beta phase in Fig. 3b as shown below.
Comments 6: Line 175. …particle strengthening effects on the hardness increment. No evidence of this result. This result can only be expressed as an assumption.
Authors response : We put supportive sentences and references in the manuscript as shown below.
“The hardness increases as the amount of EB added increases, this increment is based on the previous studies that the hardness can be increased by adding a ceramic material such as hydroxyapatite to Ti-matrix. When hydroxyapatite particles from EB added to the Ti-matrix, allowing the hydroxyapatite particles to act as a barrier to dislocations [29, 45].
[29] K. Niespodziana, K. Jurczyk, J. Jakubowicz, M. Jurczyk, Mater. Chem. Phys. 123, 160 [45] D. Bovand, M. Yousefpour, S. Rasouli, S. Bagherifard, N. Bovand, A. Tamayol, Materials & Design (1980-2015) 65, 447 (2015).
Comments 7 : Line 179. However, it depends on the fraction of b-Ti among the composites. An error should be given in determining the volume fraction of the beta phase.
Authors response : We put the right symbol in whole manuscript as “fβ”. And we defined the term as “volume fraction” in the manuscript.
“… a volume fraction of β-Ti phase (fβ) … ”
Comments 9 : Line 204. The hardness of the Ti6Al4V-EB composites increased as the EB contents increase owing to uniformly distribution of EB in the Ti6Al4V matrix. No evidence of uniformly distribution.
Authors response : Therefore, we add the figure of ball-milled composite powders with EDS area mapping result in Fig. 2 as shown below.
Comments 10 : Line 205. The composites SPSed at 1000 oC, which is beta-phase transformation temperature, showed stable elastic modulus. The research results showed that the elastic modulus varies markedly depending on the composition of the alloys. What stability modulus are the authors talking about?
Authors response : We intended that SPS temperature provide reasonable data with well-fabricated specimen, so we used the term in a wide range of meaning for “stability”, therefore, we revised the sentence to leave no misunderstanding.
“…provided well-fabricated specimens and showed reasonable mechanical properties.”
Comments 11 : Line 210. The authors suggest that additional heat treatment can decrease the elastic modulus. What article results demonstrate this effect?
Authors response : We existed reference added in the discussion part as shown below, and for this response, we found similar references.
In Page 8: “…this result showed that the proper selection of process conditions for the fabrication of Ti6Al4V matrix composites could have high strength and suitable elastic modulus for use as biomedical implants [40]. ”
Ref.
Y.T. Lee, G. Welsch Mater. Sci. Eng. A, 128 (1990) 77,
- Liu and G. Welsch: Metall. Trans. A, 19A, (1988) 1287.
Comments 12 : The article contains numerous errors showing poor English proficiency. In sum, careful work is required, both with the results obtained and with the text of the article. The article is needed major revision.
Authors response : As the reviewer’s comments, we proofread all manuscript, and figure and table captions.
All contents mentioned in this rebuttal are also addressed in the manuscript. The changes in the manuscript are highlighted in red.
With best regards,
Se-Eun Shin (Corresponding author)
Assistant Professor
Department of Materials Science and Metallurgical Engineering, Sunchon National University, Korea
E-mail: [email protected], TEL:+82-61-750-3553, FAX: +82-61-750-3550
Author Response File: Author Response.pdf
Round 2
Reviewer 1 Report
Thank you for considering the major issues proposed in my review. I hope that you will agree with me that they contribute to the qualoity and the better understanding of manuscript.
Author Response
Thank you for your comments and it helps a better quality of the manuscript before publication.
Reviewer 2 Report
The authors corrected the basic errors. However, the editing of the text is not complete. The following are typical errors encountered when reading text. After correction, the article may be accepted for publication.
Line 87, 88, 89. The powder morphologies of the starting powders, composite powders, and sintered composites were observed by using field-emission scanning electron microscopy (FE-SEM, JSM 7001F, JEOL), and energy dispersive spectroscopy (EDS) was revealed the chemical compositions of the composites.
Line 107,108. For the composites containing EB of 0.05, 0.5, and 5 wt.% has transcribed in T-0.05EB, T-0. 5EB, and 107 T-5EB, respectively.
Line 112. …cold welding could occur between the ball-milling…
Line 204. Is it a mistake? …. tricacium….
Author Response
Reviewer's comments: The authors corrected the basic errors. However, the editing of the text is not complete. The following are typical errors encountered when reading text. After correction, the article may be accepted for publication.
Authors response: We deeply apologize for these basic errors and revised carefully as shown below.
1.Line 87, 88, 89. The powder morphologies of the starting powders, composite powders, and sintered composites were observed by using field-emission scanning electron microscopy (FE-SEM, JSM 7001F, JEOL), and energy dispersive spectroscopy (EDS) was revealed the chemical compositions of the powders and the composites.
"The morphologies of the starting powders, composite powders, and sintered composites were observed...(EDS) was revealed the chemical compositions of the powders and the composites."
2. Line 107,108. For the composites containing EB of 0.05, 0.5, and 5 wt.% has transcribed in T-0.05EB, T-0. 5EB, and 107 T-5EB, respectively.
"For the composites containing EB of 0.05, 0.5, and 5 wt.% has expressed as T-0.05EB, T-0. 5EB, and 107 T-5EB, respectively."
3. Line 112. …cold welding could occur between the ball-milling…
"...occur between the balls."
4. Line 204. Is it a mistake? …. tricacium….
"...tricalcium..."
All contents mentioned in this rebuttal are also addressed in the manuscript. The changes in the manuscript are highlighted in red.
With best regards,
Se-Eun Shin (Corresponding author)
