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Article
Peer-Review Record

Wear and Abrasion Resistance of Nitride Coatings on Ceramic Substrates Processed with Fast Argon Atoms

Surfaces 2024, 7(3), 714-724; https://doi.org/10.3390/surfaces7030046
by Sergey N. Grigoriev, Alexander S. Metel *, Marina A. Volosova, Enver S. Mustafaev and Yury A. Melnik
Reviewer 1: Anonymous
Reviewer 2: Anonymous
Reviewer 3: Anonymous
Surfaces 2024, 7(3), 714-724; https://doi.org/10.3390/surfaces7030046
Submission received: 13 July 2024 / Revised: 30 August 2024 / Accepted: 2 September 2024 / Published: 4 September 2024

Round 1

Reviewer 1 Report

Comments and Suggestions for Authors

The authors' results in the surface treatment of ceramic products are exciting. Using fast argon atoms, they eliminated the defective layer to a depth of 2 to 4 µm thick. The authors report that they did not observe defects in the coatings' microstructure through the corresponding treatment. The treatment also reduced volumetric abrasive wear five times and friction wear between three and four times.

This is just an observation about your work. The first conclusion is not about your work, and therefore, I consider that it should not be included in this section as written.

Author Response

Dear Reviewer 1.

Thank you for consideration and assessment of our Manuscript. Yoy are perfecly right about the first conclusion and we excluded it from the revised Manuscript.

Reviewer 2 Report

Comments and Suggestions for Authors

Dear authors, 

overall, a well-written and interesting paper. There are just 2 comments I have.

line 34+: coatings do increase wear resistance but I would be hesitant to assign a factor (vs. uncoated). Is reduced adhesion on ceramics only  due to a "defective" outer layer ? I think adhesion of a coating is also different because of chemical bonding is different.

Second comment:

I did not understand well how you determined "density of defects" and affected depth ("thickness"). Please explain better.

Pictures / figures are good.

Sincerely

 

Author Response

Comments 1: Coatings do increase wear resistance but I would be hesitant to assign a factor (vs. uncoated). Is reduced adhesion on ceramics only due to a "defective" outer layer? I think adhesion of a coating is also different because of chemical bonding is different.

Response 1: Dear Reviewer 2.

Thank you for consideration and assessment of our Manuscript.

Of course, there are many reasons for reduction of the coating’s adhesion.

One of them is the defective surface layer. We focused on this factor and proved experimentally its important contribution.

 

Comments 2: I did not understand well how you determined "density of defects" and affected depth ("thickness"). Please explain better.

Response 2: As to the "density of defects" and affected depth ("thickness") they are determined in lines 37 – 42 of our Revised Manuscript. To explain better we should refer to [20] – Grigoriev, S.N.; Volosova, M.A.; Okunkova, A.A.; Fedorov, S.V. Influence of Defects in Surface Layer of Al2O3/TiC and SiAlON Ceramics on Physical and Mechanical Characteristics. Ceramics 2023, 6, 818–836:

“The most informative parameter that could be used to study the defectiveness of the surface layer of ceramic products is the Rt parameter which is the total height of the profile, estimated as the sum of the highest peak height of the profilogram and the most significant depth of the profile. The value of the Rt parameter allows us to take into account all possible grooves, furrows, cracks, and craters present in the surface layer and, in fact, the thickness of the defective layer.

Considering that only one parameter (Rt) is insufficient for an objective assessment of the surface layer state, we propose to evaluate the density ρ of defects (total area per unit area) on the surface of a ceramic sample in addition to it. It is proposed to use a technique based on contrasting surface defects with oblique illumination of the surface during the analysis of a stereoscopic image to assess the density of defects. The defects contrast with the main plane of the ceramic sample, where a dark color is the main plane and a light one is the surface layer defects. With the help of specialized software for image analysis (Thixomet Pro software, version 5.3.1, Saint Petersburg, Russia), the number of light pixels on the test sample is calculated. The ρ parameter value is calculated based on the data obtained for ceramic samples as the ratio of the total area of defects to the unit area of the ceramic sample under consideration.”

Thus, a new generalized criterion, “index of defectiveness” (μm), is proposed for a quantitative assessment of the defectiveness level of the ceramic product surface layer, which is determined according to the following relationship:

                                                                 Id = ρ · Rt,                                                          (1)

where ρ is the density of defects (total area) per unit area of the ceramic sample surface; Rt is the maximum profile height (thickness) of the defective layer (µm) in the considered area of the ceramic sample.

Reviewer 3 Report

Comments and Suggestions for Authors

Submitted manuscript is very interesting and it is certainly in the score of this journal. However, Authors must make some significant changes in order to insure the assecibility of this work for wide interdisciplinary audience. Title is just confusing becasuse it might be electrical resistance or wear resistance…

First of all, the quality of English is not very high and systematic style imperfection cause unfortunate difficulties for fluent readings. For example, “Application of hard films such as TiCN, DLC, TiAlN, CrAlN, TiZrN etc. on metal 34 parts increases wear resistance by about 3 times [4-6]” might be “Deposition…” or “Formation…”

The second part is related to too many technical instrumentation details which are very good to provide but – if provided – their need should be better explained in the text.  In addition, some details are given without discussion their physical/technological meaning. For example, in the Abstract we read “It is not enough for a rapid removal and a concave accelerating grid was used to decrease the beam diameter from 20 cm near the grid surface to 4.0 cm on the surface of the sample holder. It decreased the beam cross-section by 25 times and increased the sputtering rate from 0.8 μm/h to 20 μm/h.” The change of the focusing degree (beam diameter) is quite well known solution in many parts of solid state physics and technology (Nanotechnology 14 (2003) 1246–1250, https://iopscience.iop.org/article/10.1088/0957-4484/14/12/002; Procedia Engineering   184  ( 2017 )  205 – 213 doi: 10.1016/j.proeng.2017.04.087, etc.). I propose to add careful explanation to technological parts of this work with focus on the multidisciplinary audience of the journal an in a view of the existing general strategies. The abstract must be rewritten in more general style with attention to physical and technological meanings (as opposed to simply technical details).

It would be very good to add some systematic data about microstructure of the surface during all steps of the fabrication of the samples (optical microscopy, XRD, TEM) or even SEM which is present as simple illustration.

All curves must show the fitting and experimental errors must be discussed.

Comments on the Quality of English Language

The quality of English is not very high and systematic style imperfection cause unfortunate difficulties for fluent readings

Author Response

Comment 1: Submitted manuscript is very interesting and it is certainly in the score of this journal. However, Authors must make some significant changes in order to insure the accessibility of this work for wide interdisciplinary audience. Title is just confusing because it might be electrical resistance or wear resistance.

Response 1: You are perfectly right. To make the title less confusing we changed it. The title of the revised Manuscript is “Wear and abrasion resistance of nitride coatings on ceramic substrates processed with fast argon atoms”.

 

Comment 2: First of all, the quality of English is not very high and systematic style imperfection cause unfortunate difficulties for fluent readings. For example, “Application of hard films such as TiCN, DLC, TiAlN, CrAlN, TiZrN etc. on metal parts increases wear resistance by about 3 times [4-6]” might be “Deposition…” or “Formation…”

Response 2: In articles the use of “Deposition…” or “Formation…” or “Application” does not change the meaning of these convertible terms.

 

Comment 3: The second part is related to too many technical instrumentation details which are very good to provide but – if provided – their need should be better explained in the text.  In addition, some details are given without discussion their physical/technological meaning. For example, in the Abstract we read “It is not enough for a rapid removal and a concave accelerating grid was used to decrease the beam diameter from 20 cm near the grid surface to 4.0 cm on the surface of the sample holder. It decreased the beam cross-section by 25 times and increased the sputtering rate from 0.8 μm/h to 20 μm/h.” The change of the focusing degree (beam diameter) is quite well known solution in many parts of solid state physics and technology (Nanotechnology 14 (2003) 1246–1250, https://iopscience.iop.org/article/10.1088/0957-4484/14/12/002; Procedia Engineering   184  ( 2017 )  205 – 213 doi: 10.1016/j.proeng.2017.04.087, etc.). I propose to add careful explanation to technological parts of this work with focus on the multidisciplinary audience of the journal an in a view of the existing general strategies. The abstract must be rewritten in more general style with attention to physical and technological meanings (as opposed to simply technical details).

Response 3: On your advice, we rewrote the abstract in a more general style, indicating the main points of the generation and focusing the beams of fast neutral atoms and their ability to process ceramics. We agree that the change of the focusing degree (beam diameter) is quite well-known solution in many parts of solid-state physics and technology, however focusing neutral beams is a novelty and we provided some explanation of this matter.

 

Comment 4: It would be very good to add some systematic data about microstructure of the surface during all steps of the fabrication of the samples (optical microscopy, XRD, TEM) or even SEM which is present as simple illustration.

Response 4: In our work are presented data about microstructure of the sample surface obtained using optical microscopy (Fig. 12), scanning electron microscopy (Fig. 9 and Fig.10), profilometer Dektak XT (Fig. 8) and other diagnostic equipment.

Round 2

Reviewer 3 Report

Comments and Suggestions for Authors

Submitted revised version of the manuscript was improved in some way but the revision was not complete and careful.

1)      Intentionally or by misunderstanding authors did not solve the problem of the language quality. My comment is still the same: First of all, the quality of English is not very high and systematic style imperfection cause unfortunate difficulties for fluent readings. Authors should not concentrate on the particular example – careful proof-reading is necessary.  

2)      The change of the focusing degree (beam diameter) is quite well-known solution in many parts of solid-state physics and technology. Authors could add short discussion with respect to this point and describe their technology in a view of the existing techniques. It is still not clear from the current version of the text why the focusing neutral beams is a novelty and how this novelty could be used/further developed in a future.

Comments on the Quality of English Language

The quality of English is not very high and systematic style imperfection cause unfortunate difficulties for fluent readings.

Author Response

Comment 1. Intentionally or by misunderstanding authors did not solve the problem of the language quality. My comment is still the same: First of all, the quality of English is not very high and systematic style imperfection cause unfortunate difficulties for fluent readings. Authors should not concentrate on the particular example – careful proof-reading is necessary. 

Response 1. On your advice, we proofread our manuscript again and found the quality of the English to be quite high, the same as in dozens of articles we have already published in MDPI. Of course, we cannot rule out some errors, such as the one you made above: “systematic imperfection of style cause…” should be written “causes…”, since it is not plural, but singular.

 

Comment 2. The change of the focusing degree (beam diameter) is quite well-known solution in many parts of solid-state physics and technology. Authors could add short discussion with respect to this point and describe their technology in a view of the existing techniques. It is still not clear from the current version of the text why the focusing neutral beams is a novelty and how this novelty could be used/further developed in a future.

Response 2.

The focusing neutral beams is a novelty, because you can learn about it only from our publications. To our knowledge, nobody else discussed the matter. It is impossible to influence the neutral beams with electric and magnetic fields, because the fast atoms of the beam have no electric charges. When the beam is formed using a concave accelerating grid the focusing is defined with the radius of the grid surface curvature. Depending on the quality of the grid production the beam diameter in the focal point of a 20 cm diameter grid can amount to about 1 mm. Such compression of the beam is unattainable for ions and electrons. In a future our novelty could be also used for melting and evaporating materials.

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