Preparation of Silicone Coating and Its Anti-Ice and Anti-Corrosion Properties
Round 1
Reviewer 1 Report
Comments and Suggestions for Authors
Wang et al. prepared some organic silicone resin and studied their anti-icing properties.
1. The desorption time varies depending on the type of icing solution: deionized water > 5wt% NaCl of control subjects > 5 wt% NaCl. Authors should explain the reason in detail.
2. As the ice volume increases, the time required for ice melting gradually prolongs. Authors should elucidate the underlying reasons for this phenomenon in detail.
3. Authors should explain all the FTIR peaks of DMDPS, MTMS, and Silicone prepolymer in detail.
Author Response
Please see the attachment.
Author Response File: 
Author Response.docx
Reviewer 2 Report
Comments and Suggestions for Authors
In this manuscript, the authors developed organic silicone resin combining different monomers and characterized it as an anti-acing coating.
The manuscript is logically organized. However, I believe several key points require major revisions to properly address weaknesses in the technical content to strengthen the discussion and the presentation of the results.
Below are my thoughts and some detailed comments that might help revise the manuscript.
1. The materials and methods section lacks information about paragraphs 3.2 and 3.3, including subparagraphs.
2. The subheadings of section 3.3 are confusing.
3. In some cases, the description is after the related figure, and the description of Figure 7 is missing.
4. The sentence on page 2, lines 63-64, implies a consequence taken for granted.
5. The captions of the Figures 1 and 2 are incorrect.
6. In Figures 1 and 2 “Hydrolysis” and “Condensation” could be erased. In Figure 2 the specific temperature could replace “heating”.
7. The sentences on page 6, lines 209-211 are unclear and could be rephrased.
8. 9. Language needs minor revision. Many typing errors in spacing between numbers and measurement units require corrections. Some subscriptions are incorrectly smaller letters. Sodium chloride is often wrongly indicated as NaCI. The sentence on page 13 line 386 has to be erased.
9. In Figure 5 the axis and/or the name of the axis on the right should be red.
10. The errors related to all the measurements are not reported.
11. On page 325 lines 325-326 replace “melt ice” with “ice melts”.
12. On page 325, there is no correspondence between “q” in the equation and “Q” in the definition.
13. Equations should be enumerated.
14. In the Section theoretical calculation, in the Q latented definition, the multiplication and division by 1000 are not justified.
15. The conclusion in the sentences on page 12 lines 359-362 is true in general and is not well argued to support the experiments in subsections (1) and (2) (that need to be renamed).
16. The caption of Figure 11 is not clear. The blank references are missing, and the text does not clearly explain the results.
17. The sentence on page 12 lines 372-373 “However, in uncorroded areas, the coating maintains a satisfactory level of protection” is of doubtful value.
18. The caption of Figure 14 does not explain (a) and (b). What is the equivalent circuit?
19. Table 4 has to be reformatted. Moreover, some entries in it (nf, ndl) are not defined.
20. In the conclusion, what do the authors intend for “a range of silicone resin” on line 503?
Comments on the Quality of English Language
Minor editing of English language required
Author Response
Please see the attachment.
Author Response File: 
Author Response.pdf
Reviewer 3 Report
Comments and Suggestions for Authors
The article concerns research on the anti-icing properties of organic silicone resin coatings.
Comments on the article:
It is not clear what "† These authors contributed equally to this work." means. Especially since there is room in the article to include Author Contributions.
The introduction justifies the research topic and describes the current state of knowledge in the field of occurring phenomena. However, there is no reference to existing solutions to prevent these phenomena.
Materials and research methods have been described. However, there are gaps in the description of research methods. The description of electrochemical tests requires supplementation. In relation to which electrode the electrochemical corrosion parameters were determined. No studies have been described at all in 3.5wt%NaCl solution and salt spray. The base material (steel scheme) is insufficiently characterized. Don't know what steel it is? Especially since the authors further indicate the use of these coatings for galvanized or stainless steel, and the appearance after corrosion rather indicates carbon steel. The method of preparing the steel surface before applying coatings is also not described. It is an integral part of the coating production process and determines its properties. Therefore, this information must be completed.
Results
The chapter should not start with Figures. First refer to the figure in the text and then include Figures.
The structure of the text division in chapter 3.3 is confusing – (1); 1), 2) …. Etc. This note also applies to chapter 3.4.
Figure 11. How did the authors identify pitting corrosion? The photos should indicate the presence of pitting. Moreover, the local appearance of red corrosion products is not evidence of pitting corrosion. This should be better documented. Moreover, pitting corrosion and penetration of the coating into the substrate are not the same. This interpretation of the results is not understandable and requires improvement.
The phrase "Dynamic potentiodynamic" is incomprehensible (line 381).
Table 3: The sentence should start with a capital letter.
The description of the anti-corrosion mechanism should be closely correlated with the obtained test results.
In the general assessment, the test results are presented as a test report. There is no adequate discussion of the research results. There is no reference of research results to the existing state of knowledge. What new research results bring to the current state of knowledge? Furthermore, it is not fully understood how these research results relate to the anti-icing properties of these coatings.
Additionally, the title of the article indicates two aspects: (1) preparation of coatings and (2) their application to icebreakers. Both the preparation of coatings and their application are not the main focus of research in the article. Therefore, this information should not be in the title.
Author Response
Please see the attachment.
Author Response File: Author Response.pdf
Reviewer 4 Report
Comments and Suggestions for Authors
This paper studies the structure, corrosion resistance and anti-ice resistance of the hybrid organic silicon resin. The following comments may help improve the quality of the article after a minor review of the article, which is my recommendation for this publication.
Suggestions for improving the article:
1. Please change the order of the figures/tables and descriptions. First, there should be text with an explanation and reference to the figures/tables and then the figure/table - this comment does not apply to all figures/tables, but e.g., Figs. 3 and 4 are before the text. Please check and correct throughout the article to ensure that it is correct.
2. Line 176 – there is no Table 5-4 in the article. Correct the reference.
3. Add the number in brackets on the right-hand side of the sheet of each equation used.
Figure 11 - Add (a) and (b) to emphasize which figures refer to salt water resistance and which refer to salt spray resistance. Moreover, there is no reference to this figure in the text. Add it to the place where you describe it.
Author Response
Please see the attachment.
Author Response File: Author Response.docx
Round 2
Reviewer 2 Report
Comments and Suggestions for Authors
Thank you for your efforts in improving the manuscript quality. However, some critical issues still need to be resolved.
1. In the re-editing a typo error is produced in the abstract: “hermal analysis” in place of thermal analysis.
2. Saltwater resistance and salt spray resistance should be explicitly mentioned in the paragraph “Materials and methods”.
3. On page 6 Table 5-4 is introduced, but there is not in the manuscript. Is Table 1?
4. In Figures 1 and 2 “by” should be erased.
5. In the rephrased sentences on page 7, lines 233-236 be careful with spacing and replace aligning with “according to”.
6. Sodium chloride, wrongly indicated as NaCI, is still in the text (page 9 line 302) and Figure 10. Some subscriptions are incorrectly smaller letters.
7. The sentence on page 12 line 418 contains an error.
8. Equation 7 needs to be completed.
9. In the text Figure 12 is mentioned in place of Figure 11.
10. The caption of Figure 14 does not explain (a) and (b). The fact that “the “a” and the “b” in Figure 14 represent different corrosion stages, which means different corrosion routes” should be clearly explained in the text.
11. Remove the note to Table 4. Definitions in the text are sufficient.
Comments on the Quality of English Language
Minor editing of English language is required.
Author Response
Please see the attachment.
Author Response File: Author Response.pdf
Reviewer 3 Report
Comments and Suggestions for Authors
The authors have provided a revised article. The authors responded to all my comments and partially improved the article. However, the most important comments were not sufficiently corrected.
Below is my comment on the authors' responses.
1.It is not clear what "† These authors contributed equally to this work." means. Especially since there is room 4 in the article to include Author Contributions. 5
A: These authors contributed to this work means Haopeng Wang and Jihu Wang were Co-first author. 6
My comment: The authors do not understand the question. It is obvious that interchangeable people are co-authors and their contributions are given at the end of the article. So what is the purpose of this information?
2.The introduction justifies the research topic and describes the current state of knowledge in the field of occurring phenomena. However, there is no reference to existing solutions to prevent these phenomena.
A: Thanks very much for the reviewer’s suggestion. We had added some references in the Introduction.
My comment: This has been added.
3. Materials and research methods have been described. However, there are gaps in the description of research 21 methods. The description of electrochemical tests requires supplementation. In relation to which electrode the 22 electrochemical corrosion parameters were determined. No studies have been described at all in 3.5wt%NaCl 23 solution and salt spray. The base material (steel scheme) is insufficiently characterized. Don't know what steel 24 it is? Especially since the authors further indicate the use of these coatings for galvanized or stainless steel, 25 and the appearance after corrosion rather indicates carbon steel. The method of preparing the steel surface 26 before applying coatings is also not described. It is an integral part of the coating production process and 27 determines its properties. Therefore, this information must be completed. 28
A: Thanks very much for the reviewer’s suggestion. We had add detail research methods, electrochemical test methods, the technical parameters of electrochemical workstation test, 3.5wt%NaCl salt solution soaking process, and salt spray 30 resistance test expression in 2.4.
Carbon steel should be polished with 600-mesh sandpaper before use, then soaked in anhydrous ethanol and taken out after ultrasound for 2 hours, cleaned with deionized water, wiped with paper towels soaked with anhydrous ethanol, and dried with a hair dryer before scraping and coating.
The coating's fundamental physical properties were tested using instruments such as a film thickness gauge, pendulum hardness tester, pencil hardness tester, gloss meter, adhesion tester, impact strength tester, and thermal cycling chamber. The coating's freezing and desorption times were recorded using a low-temperature refrigerator, thermometer, and timer. The corrosion resistance was tested using the salt spray tank.
Before the electrochemical test, the carbon steel coated with coatings was cut, and the edge and back surface of the sample was sealed with a mixture of rosin: paraffin = 1:1. The coatings with a retention area of 1 cm ×1 cm were tested 40 using the electrochemical method. After soaking in 3.5 wt% NaCl solution for a period of time, the EIS and Tafel curves of coatings were obtained using an electrochemical workstation CHI660E, which saturated calomel electrode is used as the reference electrode, platinum electrode is used as the counter electrode, and the electrode coated with coated sample is used as the working electrode.
My comment: The research methodology has been partially completed, but there are still gaps.
There is no description of the salt spray test methodology. The results of this test are shown in Figure 11. There, the test is also called "salt spray". In the supplemented text above, the authors use the phrases: "thermal cycling chamber" and "salt spray tank". Additionally, the sentence "The corrosion resistance was tested using the salt spray tank" does not appear in the article at all. These names are wrong. The corrosion test tent should be called "salt spray test" or "salt chamber". Moreover, no data or conditions for conducting this test are provided. I believe this should be corrected and supplemented.
Results 45
4 The chapter should not start with Figures. First refer to the figure in the text and then include Figures.
A: According to reviewer’s suggestion, we had modified these mistakes and checked the full article.
My comment: This has been corrected.
5 The structure of the text division in chapter 3.3 is confusing – (1); 1), 2) …. Etc. This note also applies to 48 chapter 3.4.
A: Thanks very much for the reviewer’s suggestion. We renamed and renumbered the subsection headings. 50
My comment: This has been corrected.
6.Figure 11. How did the authors identify pitting corrosion? The photos should indicate the presence of pitting. Moreover, the local appearance of red corrosion products is not evidence of pitting corrosion. This should be better documented. Moreover, pitting corrosion and penetration of the coating into the substrate are not the same. This interpretation of the results is not understandable and requires improvement.
A: Thanks very much for the reviewer’s suggestion. We have reworded and rephrased this paragraph in response to reviewer's comments.
It is well known that steel exposed directly to 3.5 wt% NaCl will rust easily. Figure 11 shows that the prepared organo- silicon coating demonstrates a satisfactory level of corrosion resistance against 3.5 wt% NaCl and performs exception- ally well in the neutral salt spray resistance test. Pitting corrosion is observed after 168 hours in the salt spray test, likely due to minor defects on the surface of the pure resin coating, facilitating ion penetration into the substrate. Subsequently, substrate corrosion intensifies after 360 hours, leading to an overall loss of the coating’s protective properties. Both the 3.5 wt% NaCl solution immersion test and the salt spray test highlight the ability of the pure silicone resin coating to impede the penetration of corrosive agents, thereby enhancing corrosion resistance and safeguarding the metal substrate.
My comment: This comment concerned the photos presented in Figure 11. It is not clear where in these photos and on what basis the authors identify pits? The local presence of red corrosion products cannot confirm the occurrence of pitting. Pitting should be visible. Therefore, higher magnification or microscopic examination is required to confirm this.
7.The phrase "Dynamic potentiodynamic" is incomprehensible (line 381).
A: Thanks very much for the reviewer’s suggestion. We had delete the word Dynamic.
My comment: This has been corrected.
8.Table 3: The sentence should start with a capital letter.
A: According to reviewer’s suggestion, we had modified the mistake and checked the full article.
My comment: This has been corrected.
9.The description of the anti-corrosion mechanism should be closely correlated with the obtained test results.
A: Thanks very much for the reviewer’s suggestion. We had added description of the anti-corrosion mechanism. As immersion progresses into the middle and late stages, a dense layer of high-density silica forms at the substrate-medium interface, and at this point the Rct value increases dramatically.
During the whole test process, this coatings shows good anti-corrosion performance, and the salt spray resistance of the single coatings is more than 168 h. In the future, we expect it has the better performance when used together with 74 primer and intermediate paint.
My comment: The text added by the authors above does not correlate the research results with the developed mechanism. If the authors develop a mechanism, they must also indicate which study result confirms this mechanism.
10. In the general assessment, the test results are presented as a test report. There is no adequate discussion of the research results. There is no reference of research results to the existing state of knowledge. What new research results bring to the current state of knowledge? Furthermore, it is not fully understood how these 78 research results relate to the anti-icing properties of these coatings.
A: According to reviewer’s suggestion, we added some references and made minor changes to the discussion of results section. The subject of this paper is determined by the combination of corrosion and ice resistance. This part is a discussion of the tests and results conducted for corrosion resistance, while ice resistance is realized mainly due to the low surface energy of the silicone resin itself. That is the reason why we chose this material.
My comment: The supplemented text is not a discussion of the research results obtained in relation to the existing state of knowledge.
11.Additionally, the title of the article indicates two aspects: (1) preparation of coatings and (2) their application to icebreakers. Both the preparation of coatings and their application are not the main focus of research in the 86 article. Therefore, this information should not be in the title.
A: According to reviewer’s suggestion, the title was changed to Preparation and anti-icing properties of organic silicone resin coatings.
My comment: The title of the article has been changed.
Author Response
Please see the attachment.
Author Response File: Author Response.pdf
