Wear Behavior of TiN/TiAlSiN Nanocomposite Multilayer Coatings from Ambient Temperature to Medium Temperature
Round 1
Reviewer 1 Report
Comments and Suggestions for AuthorsThe manuscript reports on manufacturing of composite coatings on metallic substrate and comprehensive study of chemical and mechanical properties of resulting material. I found this manuscript well suited to the topic of the journal and to be of practical importance. The material has been well studied using a range of methods including FE-SEM+EDS, XRD, XPS and mechanical tests. Nevertheless some extensive textual correction is required to improve the readability of the manuscript.
1) Line 17 ‘from TiN 111 to Ti3AlN 111 after ’, should be ‘from TiN (111) to Ti3AlN (111) after ’
2) Lines 89-91: ‘TiN/TiAlSiN multilayer coatings were deposited on titanium alloy TA15 as outlined 89 in Table 1 for its composition using multi-arc ion plating equipment (JGP-800). The TiAlSi 90 (55:35:10) alloy target ’ Please, specify the manufacturer of JGP-800 device. Please specify the manufacturer of substrate and target materials. How the composition (table 1) of the TA15 substrate was measured?
3) line 110: ‘D8 Advance X-110 ray diffractometer (XRD) patterns. ’ Specify the manufacturer of diffractometer. Was it Bruker D8 Advance?
4) Please add experimental details on heat-treatment of sample at 500ºC after deposition to experimental section. Specify the heating and cooling mode, gas atmosphere etc.
5). Figure 1: a) add the line and mark the direction of line scan on ‘a’ panel
b) the expected scheme of layers (depicted as colored bars) in the sample below the line-scan on panel ‘b’ to allow readers to compare experimental composition with expected one.
c) modify the caption of figure ‘Figure 1. Cross-sectional morphology of TiN/TiAlSiN multilayer coating: (a) SEM morphology, (b) cross-section line scan, (c) layer â… - the Ti buffer layer point scan, (d) layer â…¡- the TiN layer point scan, (e) layer â…¢-the TiAlSiN layer point scan. ’
6) lines 184-185 ‘changed from TiN 111 to Ti3AlN 111 after oxidation test. Also the orientation of Ti3AlN shift from 200 to 111. ’ Please use brackets () for Miller indexes – (111), (200) etc. To confirm the change of the orientation please calculate the texture coefficients. Registration of the Pole Figure would be more reliable confirmation of this effect.
Comments on the Quality of English Language
The manuscript requires minor text editing to improve readability.
Author Response
The authors would like to express their gratitude to the reviewers for their valuable comments. We have diligently considered their feedback and made improvements to the work, specifically addressing the concerns highlighted below.
Comments from reviewer 1
The manuscript reports on manufacturing of composite coatings on metallic substrate and comprehensive study of chemical and mechanical properties of resulting material. I found this manuscript well suited to the topic of the journal and to be of practical importance. The material has been well studied using a range of methods including FE-SEM+EDS, XRD, XPS and mechanical tests. Nevertheless some extensive textual correction is required to improve the readability of the manuscript.
- Line 17 ‘from TiN 111 to Ti3AlN 111 after ’, should be ‘from TiN (111) to Ti3AlN (111) after ’
Response: It has now been revised and marked in red in the manuscript.
2) Lines 89-91: ‘TiN/TiAlSiN multilayer coatings were deposited on titanium alloy TA15 as outlined 89 in Table 1 for its composition using multi-arc ion plating equipment (JGP-800). The TiAlSi 90 (55:35:10) alloy target ’ Please, specify the manufacturer of JGP-800 device. Please specify the manufacturer of substrate and target materials. How the composition (table 1) of the TA15 substrate was measured?
Response: We have added the manufacturer of multi-arc ion plating equipment, target and substrate and marked in red in the manuscript. “The TA15 substrate was produced by the Beijing Institute of Aviation Materials, and its corresponding chemical composition is detailed in Table 1.” The composition of TA15 is provided by the institute, not by our measurement.
3) line 110: ‘D8 Advance X-110 ray diffractometer (XRD) patterns. ’ Specify the manufacturer of diffractometer. Was it Bruker D8 Advance?
Response: Yes, it is Bruker. We have added the manufacturer and rewrite the sentence.
The phase structure analysis of the TiN/TiAlSiN multilayer coatings was conducted using a Bruker D8 Advance X-ray diffractometer (40 kV, 30 mA, Cu K radiation (λ = 0.154 nm)).
4) Please add experimental details on heat-treatment of sample at 500ºC after deposition to experimental section. Specify the heating and cooling mode, gas atmosphere etc.
Response: We have added the required information and marked in red.
The samples underwent thermal treatment in a muffle furnace under an air atmosphere, where they were heated to 500 ℃ at a heating rate of 10 K/min and maintained at this temperature for 10 hours. This was followed by a cooling process at a rate of 50 K /min, conducted without preservation.
5). Figure 1: a) add the line and mark the direction of line scan on ‘a’ panel
- b) the expected scheme of layers (depicted as colored bars) in the sample below the line-scan on panel ‘b’ to allow readers to compare experimental composition with expected one.
- c) modify the caption of figure ‘Figure 1. Cross-sectional morphology of TiN/TiAlSiN multilayer coating: (a) SEM morphology, (b) cross-section line scan, (c) layer â… - the Ti buffer layer point scan, (d) layer â…¡- the TiN layer point scan, (e) layer â…¢-the TiAlSiN layer point scan. ’
Response: We have added the line scan direction in Figure 1a, the layers scheme in Figure 1b and modified the caption and marked in red.
Figure 1. Cross-sectional morphology of TiN/TiAlSiN multilayer coating: (a) SEM morphology, (b) cross-section line scan, (c) layer â… -the Ti buffer layer point scan, (d) layer â…¡- the TiN layer point scan, (e) layer â…¢-the TiAlSiN layer point scan.
6) lines 184-185 ‘changed from TiN 111 to Ti3AlN 111 after oxidation test. Also the orientation of Ti3AlN shift from 200 to 111. ’ Please use brackets () for Miller indexes – (111), (200) etc. To confirm the change of the orientation please calculate the texture coefficients. Registration of the Pole Figure would be more reliable confirmation of this effect.
Response: Thank you for your suggestion. We have added the brackets and the calculation of texture coefficient and marked in red. While we have opted not to include the Pole Figure in this study due to resource constraints and the focused scope of our research. We believe that the texture coefficients sufficiently support our conclusions. We appreciate your understanding.
Table 3 Texture coefficient of TiN/TiAlSiN multilayer coating before and after oxidation
|
Peak position |
Planes(hkl) |
TC (before oxidation) |
TC (after oxidation) |
|
38.07 |
(111) |
2.67 |
0.43 |
|
43,7 |
(200) |
0.53 |
1.84 |
|
63.7 |
(220) |
0.43 |
1.03 |
|
76.83 |
(311) |
0.37 |
0.7 |
Author Response File: 
Author Response.pdf
Reviewer 2 Report
Comments and Suggestions for AuthorsThank you for your work.
Please find my comments below. Additionally, I have inserted some comments in the sidebar of the PDF file.
- Punctuation and commas need revision.
- Please define or specify the ambient temperature if possible.
- Please discuss the effect of oxidation on the wear rate.
- The caption for Figure 5 does not include descriptions for sub-figures d, e, and f.
- The captions of most figures need to be extended. For example, Figure 8 does not contain explanations for the sub-figures.
- Please improve the SEM and simulation figures by increasing the aspect ratio (w/L) and resolution.
- The author does not present the initial specimen conditions. The configuration and dimensions of the specimens used should be included if relevant to the experiments, along with the standards used. Additionally, details of the experiments, such as polishing, should be provided.
- The equations throughout the manuscript do not have numbers. In addition, please refer to these equations when making comparisons with your experiments.
Regards
Comments for author File: Comments.pdf
Author Response
The authors would like to express their gratitude to the reviewers for their valuable comments. We have diligently considered their feedback and made improvements to the work, specifically addressing the concerns highlighted below.
Reviewer 2
Please find my comments below. Additionally, I have inserted some comments in the sidebar of the PDF file.
comment 1: Punctuation and commas need revision.
Response: Thank you for this suggestion. We have checked the punctuation and commas.
comment 2: Please define or specify the ambient temperature if possible.
Response: Thank you for suggestion. Usually in simulation, ambient temperature is typically considered to be between 20 and 25 ℃. In Section 2.3, we have specified the ambient temperature as 25 °C.
comment 3: Please discuss the effect of oxidation on the wear rate.
Response: We discussed the wear rate after oxidation in Section 3.6.2.
In Figure 8d-e, it is evident that sintered debris adheres to the wear track and, in certain areas, attains a higher height than the coating itself. This presence of oxide within the debris contributes to an overall increase in debris volume, rendering it challenging to accurately quantify the wear loss.
comment 4: The caption for Figure 5 does not include descriptions for sub-figures d, e, and f.
Response: Sorry for this error, we have labeled the right one and marked in red in the manuscript.
Figure 5. SEM images and 3D profiles of the wear tracks of the substrates and the coated samples at different temperatures: substrate at (a) room temperature (RT), (b) 300 ℃, and (c) 500℃; coated sample at (d) RT, (e) 300 ℃, and (f) 500℃.
comment 5: The captions of most figures need to be extended. For example, Figure 8 does not contain explanations for the sub-figures.
Response: Thank you for this suggestion. we have added the detailed information of the Figure 8 and marked in red as shown below. We also examined other images.
Figure 8. SEM, EDS result and 3D profile of the wear track of the coated sample oxide in 500 ℃ for 10 h.
(a) SEM of wear track morphology, (b) enlarged image of the red box in Figure 8a, (c) the composition of two types of debris and the coating surface after oxidation, (d) 3D morphology, (e) the depth profile of the wear track.
comment 6: Please improve the SEM and simulation figures by increasing the aspect ratio (w/L) and resolution.
Response: we have modified the Figure 8 followed this suggestion.
comment 7: The author does not present the initial specimen conditions. The configuration and dimensions of the specimens used should be included if relevant to the experiments, along with the standards used. Additionally, details of the experiments, such as polishing, should be provided.
Response: we have added the information about TA15 and the grounding and polishing details.
The TA15 substrate was produced by the Beijing Institute of Aviation Materials, and its corresponding chemical composition is detailed in Table 1. The substrates with a dimensions of 15 mm×15 mm×4 mm were grounded by SiC abrasive paper from 150 grit to 7000 grit, and subsequently polished using chromic oxide. The polished samples were ultrasonically cleaning in alcohol for 10 min to eliminate surface contamination.
comment 8: The equations throughout the manuscript do not have numbers. In addition, please refer to these equations when making comparisons with your experiments.
Response: Thanks for the suggestion, we have added the number and refer to the equations.
Table 5 provides the corresponding details and quantifications of wear volume and wear rate, with the wear rates calculated using equations (1) and (2).
Author Response File: Author Response.pdf
Reviewer 3 Report
Comments and Suggestions for AuthorsThe work is interesting, although classic if you put its subject matter. The work should be organized so that it is clearer whether the results are for tribological studies at elevated temperatures or at room temperature after oxidation. It seems that the results of post-oxidation friction and analysis of the results for the oxidation of an uncoated titanium alloy sample are not included. In this regard, the article could be supplemented which would allow broader conclusions. It is necessary to remove from the reported values, those ranges that are within the error range with respect to the results of microanalysis of chemical composition or microhardness, for example. E.g., giving the microhardness result with the accuracy of a decimal fraction is a big mistake.
Author Response
The work is interesting, although classic if you put its subject matter. The work should be organized so that it is clearer whether the results are for tribological studies at elevated temperatures or at room temperature after oxidation. It seems that the results of post-oxidation friction and analysis of the results for the oxidation of an uncoated titanium alloy sample are not included. In this regard, the article could be supplemented which would allow broader conclusions. It is necessary to remove from the reported values, those ranges that are within the error range with respect to the results of microanalysis of chemical composition or microhardness, for example. E.g., giving the microhardness result with the accuracy of a decimal fraction is a big mistake.
Response: Thank you for the valuable suggestions.
- The wear test was conducted at room temperature following oxidation. We added details at section 3.6.2, as presented below:
3.6.2 Wear behavior at room temperature subsequent to oxidation
- Thank you for your valuable feedback regarding the inclusion of post-oxidation friction results for the uncoated titanium alloy sample. However, due to time constraints and the primary focus of our study on the coatings, we have decided not to include this data. We believe that concentrating on the coatings will provide more relevant insights for our research objectives. We appreciate your understanding."
- We remove the decimal fraction when mentioned microhardness and added the error in the table. As shown below
Table 3 Micro Vickers hardness of TA 15 and TiN/TiAlSiN multilayer coating
|
Position |
1/HV0.1 |
2/HV0.1 |
3/HV0.1 |
4/HV0.1 |
5/HV0.1 |
average/HV0.1 |
|
TA15 |
386 ± 0.9 |
342 ± 0.6 |
326 ± 0.5 |
356 ± 0.5 |
341 ± 0.4 |
350.2 ± 0.5 |
|
TiN/TiAlSiN |
1533 ± 1.8 |
1717 ± 2.4 |
1485 ± 2.7 |
1426 ± 1.5 |
1541 ± 2.8 |
1540 ± 2.2 |
As seen in Table 3, the average micro Vickers hardness of the TA15 titanium alloy substrate is 350 HV0.1, while the average hardness of the TiN/TiAlSiN multilayer coating is 1540 HV0.1, which is 5 times higher than that of the substrate.
Author Response File: Author Response.pdf
