Vapor–Gas Deposition of Polymer Coatings on Metals from Azeotropic Solutions of Organosilanes

Round 1

Reviewer 1 Report

In this research, a new method of vaporgas deposition of powder inhibitors on metals is proposed, which makes it possible to obtain composite coatings with VS and volatile corrosion inhibitors. The chemical compositions of siloxane coatings were determined with the help of XPS and the mechanisms of interaction of VS with polymerization promoters ethylene glycol (EG) and 1,1-diphosphonic acid (DPA) were propose. However, before the paper can be accepted, the following issues need to be addressed.

1. On page 9, Sentence “Preliminary studies have shown that no precipitate is formed during the evaporation of BTA and DPA solutions, i.e. the inhibitors are completely evaporated during vapor deposition” needs to be marked with citations;

2. When citing references in the same category, the format needs to be uniform, and the author should carefully check and revise this;

3. There are some formatting problems in the body of the paper, such as Figure 7, Fig. 8, etc., and the author needs to modify them;

4. On page 9, “The thickness of the VS coatings with additives EG, DPA and BTA was 450, 210 and 120 nm, respectively”. How the thicknesses of these coatings are calculated;

5. In Figure 4, the authors need to distinguish between test curves, fitted curves, and baselines;

6. The English writing of the full text needs to be improved.

The English writing of the full text needs to be improved.

Author Response

1. Preliminary studies were conducted within the framework of this work, so there is no one to quote.
2. It is not entirely clear what “references in the same category” is

      3.Figure 7 has been corrected

4. The thickness of the coatings was determined by calibration curves obtained by XPS ion etching, added to the experimental methodology.
5. In Figure 4, the experimental data are indicated by dots. Fitted with a solid line . They do not differ well, since this spectrum is singlet with a good signal intensity.
6. The text has been re-edited.

Reviewer 2 Report

The manuscript should be rejected because its level is far from the gate of being reviewied. The author should have asked his colleagues to carefully examine and check the manuscript. According to the references, he previously published several papers [12], [13] and [14] with other people. So that he could have found several kind and intelligent researchers.

The author should have examined the word by word, sentence by sentence, line by line and paragraph by paragraph before the submission of the manuscript. Furthermore, it contains many miss-typing and English errors. 

The author must be very careful of being strictly logical in writing a scientific paper otherwise a reviewer would give up following the research story.

The next version, if it would be created, should be checked by an English-native beforehand.

Author Response

Responses to comments

Dear Dr. Yuri makarychev, Congratulation! Your nominated profile has been selected for the "International Research Awards on Composite Materials" under the category of "Best Researcher Award". Your Entry Id is 8903.

Author Response File: Author Response.docx

Reviewer 3 Report

In this work, a new method of vapor-gas deposition of powder inhibitors on metals is proposed, which makes it possible to obtain composite coatings with vinyltrimethoxysilane and volatile corrosion inhibitors. To some extent, this is a topic of interest to the researchers in the related areas and this paper can be published after some minor revisions. The following points require consideration:

(1)   The abstract is too long. Reformulate the abstract in order to clearly show the strengths of this work.

(2)   Quantitative information is not provided in the abstract.

(3)   Some sentences need reconstruction and the level of English should be improved.

(4)   Please highlight the advantages and disadvantages of the developed method.

Author Response

. The abstract has been corrected.

2. Quantitative information is provided in the abstract
3. The text was re-edited.
4. The advantages of the proposed method are described in the introduction and in section 4 discussion

Reviewer 4 Report

Manuscript ID: surfaces-2539297 entitled:

Vapor-gas deposition of polymer coatings on metals from azeotropic solutions of organosilanes

Authors

Yuri Borisovich Makarychev

General comment

This paper presents the results of the study regarding vapor-gas deposition of vinyltrimethoxysilane (VS) from azeotropic solutions. A new method of vapor-gas deposition of powder inhibitors on metals is proposed, in order to obtain composite coatings with VS and volatile corrosion inhibitors.

Some recommendations and observation remain:

1. In experimental part at pg 3 complete the missing words in the phrase:

 “To calculate the thicknesses of the layers, the values of electron free path lengths (or average attenuation coefficients calculated by…”3.

2. At pg 4 insert in figure 1 the OY axe (% transmittance) for VP compound.

3. The experimental part must be more concise. Read carefully the text. It is not clear why phenol appear in discussion. Phenol is not mentioned in materials at the beginning and why is present. This need to be explained.

4. The figure 7 must be revised, some atoms of carbon present five or three bonds.

5. In table 3 IPS is  used, but in material section this  compound is not abbreviated. Mention the necessity of using IPS and the necessary amount.

6. Insert a table with an experimental data for the prepared coatings (with their notation, composition, deposition conditions and thickness).

7. It would be beneficial to include SEM images of the prepared coatings. The morphology (compactness) of the coatings correlated with the XPS data is also beneficial and edifying.

Author Response

Responses to comments.

1. corrected
2. corrected
3. Changes were made to the Experimental section
4. corrected
5. Fixed
6. The modes of coating deposition are given in Table 3 and the thickness of coatings in Fig.6.
7. The equipment available to us does not currently allow us to examine the morphology of the coatings with such a high resolution < 0. 1 μm.

Author Response File: Author Response.docx

Reviewer 5 Report

Comments of surfaces-2539297

The main weaknesses of the manuscript:

1.     The abstract can be improved to show more significance and findings of study.

2.     It is suggested that the conclusion should be expressed more clearly and methodically.

3.     Please add references from the last five years.

4.     The discussion points for XPS images are not well supported with other literature findings.

5.     %at need to change to at.%.

Comments for author File: Comments.docx

Author Response

1.The abstract has been corrected

2.Conclusions have been modified.

3.The deposition of polymer coatings on metals from vapor phase organosilanes is a new field developed by us in the last two years. Therefore, there is no literature data in this research area.

4. In the text there are references to our works, where detailed interpretations of these spectra are presented.

Round 2

Reviewer 2 Report

Improvements have been made over the first version. However, there still remain several points to be improved.

1. Concerning on "metals" in the title and "iron" in the conclusions. The author seems to be insensible to materials used for his research. The specimen metal was carbon steel of St.3, right? (Paragraph 2.2) Is this a steel of Russian standard? What are its chemical composition and the metallographic structure? How was the specimen prepared for the azeotropic coating? By the way, "iron" is the name of an element.

2. In this version, the author does not describe the experimental setup for the coating. How was the mixture of chemicals heated to evaporate on the surface of the steel specimens? How were the reduced evaporation temperatures measured? How much was the specimen temperature?

3. The author uses abbreviations for chemicals too frequently. At least in the "Conclusions", both expressions should be written for clarity.

3. This research article does not have no "Discussion" section. The author writes in the abstract as follows; "which allows to reduce the evaporation temperature .........", and also "A new method of vapor-gas deposition of..........." These statements need detailed explanation along with [15].

4. As to the references, [15] is cited after [19]. This is strange. The URL for [15] should be added so that the readers can read and evaluate this research.

Nothing.

Author Response

1. The composition of the steel is given in p. 2.2. Preparation of the sample before deposition of coatings is given in p.2.2. “Iron" is corrected on St.3
2. A diagram of an experimental setup with a method for determining the temperature of the sample and the evaporator is given.
3. Changes have been made to the Conclusions .
4. Added section 4 Results and discussion
5. Changes have been made to the literature section. The URL is unknown to me. Data on the boiling points of azeotropic mixtures can be found in Wikipedia https://ru.wikipedia.org " wiki "

Author Response File: Author Response.docx

Reviewer 4 Report

Manuscript ID: surfaces-2539297 entitled:

Vapor-gas deposition of polymer coatings on metals from azeotropic solutions of organosilanes

Authors

Yuri Borisovich Makarychev

General comment

This paper presents the results of the study regarding vapor-gas deposition of vinyltrimethoxysilane (VS) from azeotropic solutions. A new method of vapor-gas deposition of powder inhibitors on metals is proposed, in order to obtain composite coatings with VS and volatile corrosion inhibitors.

Some recommendations and observation remain:

1.       I did not find the author's answers in the text. for example, comment 3, to understand figure 2 and table 3

2.        At pg 4 insert in figure 1 the OY axe (% transmittance) for VP compound in detail image.

3.       Regarding comment 6, the suggestion was for a better understanding and centralization of the experimental data (Insert a table of experimental data for the prepared coatings (with their notation, composition, deposition conditions and their thickness). The author replies "The ways of layer deposition are given in Table 3 and the thickness of the coatings in Fig.6.” but Fig. 6 does not give the thickness.

Author Response

1. Fixed
2. In Fig. 1 and other optical spectroscopy spectra, the names of all axes are checked. There are no violations.
3. Changes have been made to the Experimental part section
4. Fixed
5. Fixed
6. The deposition modes of coatings are shown in Table 4, and the thickness of coatings in Fig.11
7. The equipment we have does not currently allow us to study the morphology of coatings with such a high resolution < 0.1 microns.

Author Response File: Author Response.docx

Round 3

Reviewer 4 Report

Author's response to report 1 has 7 comments. For report 2, there were 3 comments but the answer is identical to that of report 1. I ask the author to send the answers for report 2.

 Also, phenol is toxic, is its use a viable solution?

Author Response

Response to the comments of paragraphs 1 and 2 .

Figure 4 (1 version of the article) or Figure 2 (2 version of the article) shows the XPS spectra, not optical. The intensity of the photoelectronic spectrum is indicated on the y-axis. The names of the other axes in all the figures have been repeatedly checked. There are no violations. Phenol has been added to the list of reagents of the experimental part. Phenol is chosen because of the known solvents gives the lowest boiling point of the azeotropic mixture. In the following works we will look for a replacement. Table 7 with compositions, application conditions and coating thickness has been added to the text of the article.