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Article
Peer-Review Record

Preparation and Properties of Conductive Aluminum Powder (Al@Si@C) for Water-Borne Heavy-Duty Anticorrosive Coatings

Coatings 2024, 14(9), 1082; https://doi.org/10.3390/coatings14091082
by Qingpeng Li 1,2,*, Jiaxing Liu 1, Tiancheng Jiang 1, Xiaoyun An 1, Na Wang 1,2, Zhixiu Xu 3, Wanyuan Guo 3, Liang Zhang 4 and Xiaofeng Liu 1,*
Reviewer 1:
Reviewer 2: Anonymous
Reviewer 4: Anonymous
Coatings 2024, 14(9), 1082; https://doi.org/10.3390/coatings14091082
Submission received: 28 June 2024 / Revised: 9 August 2024 / Accepted: 20 August 2024 / Published: 23 August 2024

Round 1

Reviewer 1 Report

Comments and Suggestions for Authors

The authors studied the deposition of aluminium coating containing different contents of Si and carbon powder on mild steel for water-borne heavy-duty anticorrosive coating applications.

The experimental works are very interesting and the findings of the outcomes research result in optimal composition of Al-Si with 5% C. However, the reviewer does not find in the experimental procedure, mentioning briefly how to obtain: the resistivity test, storage stability test,  polarization test, hydrogen evolution test as shown in Fig. 11, and neutral salt spray test in Figs. 15 and 16 in the section of #2.  FT-IR, XPS, XRD, and EDS are used for characterizations of samples after Al-Si-S depositions. The specific properties of Al-Si-C depositions on mild steel matching a requirement for heavy-duty anticorrosive coating application are not mentioned in the manuscript. Therefore, the reviewer highly recommends the authors for highlighting the gap and significance of the research. In addition, the objective of the research specifically should be mentioned in the section of the last paragraph.

Results and discussion: The reviewer strongly recommends the authors confirm and compare the chlorine corrosion (5%NaCl) inducing Al-Si-C coating on mild steel surfaces. At least 5 papers the authors cite from the closest experimental research available in the literature. In addition, Fig. 16 displays the surface of metal corrosion that needs to be observed by SEM for a deep discussion of how chloride corrodes the coating surface. Please provide deeply comprehensive discussions in each section for data obtained from test results. What are the significant findings obtained from the present experimental works compared to previous research available in the literature?

 

In the conclusion section: the authors should highlight the significant findings of the research outcomes that respond to the research objective mentioned in the introduction section. What are the beneficial contributions from the findings of the research for water-borne heavy-duty anticorrosive coating application?

Author Response

Comments 1:[The experimental works are very interesting and the findings of the outcomes research result in optimal composition of Al-Si with 5% C. However, the reviewer does not find in the experimental procedure, mentioning briefly how to obtain: the resistivity test, storage stability test, polarization test, hydrogen evolution test as shown in Fig. 11, and neutral salt spray test in Figs. 15 and 16 in the section of #2.  FT-IR, XPS, XRD, and EDS are used for characterizations of samples after Al-Si-S depositions. The specific properties of Al-Si-C depositions on mild steel matching a requirement for heavy-duty anticorrosive coating application are not mentioned in the manuscript. Therefore, the reviewer highly recommends the authors for highlighting the gap and significance of the research. In addition, the objective of the research specifically should be mentioned in the section of the last paragraph.

Results and discussion: The reviewer strongly recommends the authors confirm and compare the chlorine corrosion (5%NaCl) inducing Al-Si-C coating on mild steel surfaces. At least 5 papers the authors cite from the closest experimental research available in the literature. In addition, Fig. 16 displays the surface of metal corrosion that needs to be observed by SEM for a deep discussion of how chloride corrodes the coating surface. Please provide deeply comprehensive discussions in each section for data obtained from test results. What are the significant findings obtained from the present experimental works compared to previous research available in the literature?]

Response 1: [Our group has conducted an in-depth discussion and analysis on the questions you raised, and we all agreed that the questions you raised are very constructive and provide ideas for our further research work.

According to your advice, the experimental procedure of Al-Si with 5% C has been supplemented in the part of “2.2.3. Preparation of Conductive Aluminum Powder” (Page 3, lines 139-140).

According to your advice, the relevant literature is cited, and the research progress and difficulties are analyzed, and the research objectives are proposed in the last paragraph of “1. Introduction”, as “In order to solve the application bottleneck of aluminum powder in water-borne heavy anticorrosive coatings and to effectively resolve the hydrogen precipitation problem of the aluminum powder in the aqueous system” (Page 3, lines 101-103).

This paper focuses on the surface modification of aluminum powder, and concentrates on the storage stability of aluminum powder in water-borne system and the electrical conductivity of aluminum powder. This paper is the first part of a series of studies on water-based aluminum coatings. In the future, we will focus on studying the effect and mechanism of modified aluminum powder on corrosion resistance of coatings.]

Comments 2:  [In the conclusion section: the authors should highlight the significant findings of the research outcomes that respond to the research objective mentioned in the introduction section. What are the beneficial contributions from the findings of the research for water-borne heavy-duty anticorrosive coating application?]

Response 2: [Thank you for your valuable advice. The beneficial contributions from the findings of the research are depicted in the last paragraph of “4. Conclusion”, as “Therefore, the prepared conductive aluminum powder possessed excellent electrical conductivity and corrosion resistance, effectively solving the hydrogen evolution stability of aluminum powders in water-based coating systems and broadening the applications of water-borne coatings in anti-corrosion fields” (Page 17, lines 569-572).]

Reviewer 2 Report

Comments and Suggestions for Authors

The topic presented in the manuscript entitled "Preparation and Properties of Conductive Aluminum Powder (Al@Si@C) for Water-borne Heavy-duty Anticorrosive Coatings" is very interesting, but the quality of the presentation of the information could be improved for better presentation and easier understanding by the reader. 

The section on the description of the experiment (2.2. Experiments) could be presented in graphical form, e.g. a diagram/scheme. 

The title of section 2.4 needs to be clarified; to me it is inadequate. 

The text lacks information on the procedure for taking SEM photographs, which is relevant to the topic under consideration. 

What would you say is the procedure for preparing samples for SEM photography?

Additional details on the SEM setup are recommended. For example, what accelerating voltage was used?

What type of detector was used to image the materials produced? Secondary electron detector?

Additional details of the SEM settings are recommended. For example, what accelerating voltage was used?

For Figures 6 and 12, it is recommended that the dimensions of the field of view or the size of the scale are given.  

The quality of Figure 13 needs to be improved. Why was wettability measured with one measuring liquid?

Furthermore, in Figure 13 C the measuring liquid has evidently spilled, so surely the result is reliable?

Perhaps conclusions in point form would be clearer. I leave this comment for the authors to consider. 

Author Response

Comments 1: [The topic presented in the manuscript entitled "Preparation and Properties of Conductive Aluminum Powder (Al@Si@C) for Water-borne Heavy-duty Anticorrosive Coatings" is very interesting, but the quality of the presentation of the information could be improved for better presentation and easier understanding by the reader.]

Response 1: [Thank you for your suggestion to this work. The quality of the presentation of the information has been revised by a professional teacher according to your advice. There are more modifications, please see the highlights in the manuscript.]

Comments 2: [The section on the description of the experiment (2.2. Experiments) could be presented in graphical form, e.g. a diagram/scheme.]

Response 2: [Thank you for your suggestion. The section of the modification process of aluminum powder (2.2. Experiments) is relatively complex, and cannot be comprehensively expressed using the graphical form, so the form of words is chosen to elaborate.]

Comments 3: [The title of section 2.4 needs to be clarified; to me it is inadequate.]

Response 3: [Thank you for your valuable advice. The title of section 2.4 has been modified into “2.4. Characterization Methods” (Page 6, line 197).]

Comments 4: [The text lacks information on the procedure for taking SEM photographs, which is relevant to the topic under consideration. What would you say is the procedure for preparing samples for SEM photography? Additional details on the SEM setup are recommended. For example, what accelerating voltage was used? What type of detector was used to image the materials produced? Secondary electron detector? Additional details of the SEM settings are recommended. For example, what accelerating voltage was used?]

Response 4: [Thank you for your valuable advice. The equipment and procedure information related to SEM has been perfected, as “The morphology and energy spectrum mapping of the samples were performed using scanning electron microscope (SEM) (ZEISS Gemini SEM 300, Germany) supplemented with energy dispersive spectrometer (EDS). The powder sample was glued to the conductive adhesive, and then sputtered with a gold layer by Quorum SC7620 sputtering coater with 10 mA power supply. The acceleration voltage was 3 kV for topography shooting and 15kV for energy spectrum mapping with SE2 secondary electronic detector” (Page 6, lines 200-205).]

Comments 5: [For Figures 6 and 12, it is recommended that the dimensions of the field of view or the size of the scale are given.]

Response 5: [Thank you for your suggestion. The scale bar in Fig. 6 (Page 8, line 301) and Fig. 12 (Page 13, line 441) has been modified.]

Comments 6: [The quality of Figure 13 needs to be improved. Why was wettability measured with one measuring liquid?]

Response 6: [Thank you for your suggestion. The modified aluminum powder studied in this paper will eventually be applied to water-borne coatings, so the hydrophilicity of the modified powder is used to investigate its dispersion in water, so only water is used to measure the wettability.]

Comments 7: [Furthermore, in Figure 13 C the measuring liquid has evidently spilled, so surely the result is reliable?]

Response 7: [Thank you for your suggestion. The hydrophilicity of the modified aluminum powder is improved, which led to the result as shown in Figure 13C. This was not a phenomenon of liquid spill, but a result of better wettability and smaller contact angle after the improvement of hydrophilicity.]

Comments 8: [Perhaps conclusions in point form would be clearer. I leave this comment for the authors to consider.]

Response 8: [Thank you for your suggestion. There are two conclusions in this paper, which are summarized in two paragraphs according to your comments (Page 16-17, lines 550-571).]

Reviewer 3 Report

Comments and Suggestions for Authors

The article Preparation and Properties of Conductive Aluminum Powder (Al@Si@C) for Water-borne Heavy-duty Anticorrosive Coatings, is well written, the prepared materials were characterized by various methods to demonstrate that the aluminum powder was successfully modified with Si and C and that there were dense films of SiO2 and nanoconductive carbon black on the surface of the aluminum powder. Resistance measurements demonstrated that the resistivity of the conductive aluminum powder was reduced compared to that of the SiO2-modified aluminum powder, indicating a significant improvement in electrical conductivity.

 I recommend moving table 1 to the next page to make it easier to study.

It is a complex article and I think it can be published

Author Response

Comments 1: [I recommend moving table 1 to the next page to make it easier to study.]

Response 1: [Thank you for your recognition and suggestion to this work. Table one has been moved to a page (Page 9, lines 314-315).]

Reviewer 4 Report

Comments and Suggestions for Authors

Authors need to provide the XRD patterns of powders  vs coated samples to better understand of the prepared coating materials.

Please index the FTIR bands in Fig. 4 and discuss the signficance of there existence? 

In Fig.6, scale bar is not visible, please rescale it.

Al, O and C elemental XPS spectrum are need to add and discuss in revised manuscript. 

what is relationship of H2 yield vs corrosive protective coatings? please specify clearly.

EIS spectra of the materials need to study in deepth and discuss the details of EIS spectra in revised manuscript. 

for sake of competence and improve the readership of this article, authors refer and cite these articles in introduction part: RSC advances 14 (20), 14263-14277;  Materials 202417(1), 126; https://doi.org/10.3390/ma17010126;  Alexandria Engineering Journal 59 (6), 4449-4462; Coatings 202111(4), 453; https://doi.org/10.3390/coatings11040453

There are several typo and format errors, please revise

Author Response

Comments 1: [Authors need to provide the XRD patterns of powders vs coated samples to better understand of the prepared coating materials.]

Response 1: [Thank you for your suggestion. The focus of this paper is not on the coating is not the coating but the modified aluminum powder sample, and the coating is our next research content. Furthermore, the purpose of the XRD characterization is to prove that the crystal structure of Al powder is not changed after modification, so that the sacrificial anode effect in the coating is not be affected. Therefore, we thought it was no necessary to characterize the coating by XRD in this paper.]

Comments 2: [Please index the FTIR bands in Fig. 4 and discuss the signficance of there existence?]

Response 2: [Thank you for your valuable advice. The spectrum of carbon black in Fig. 4 is compared and basically consistent with the theoretical spectrum in the spectrum library. So far, there are few studies on KH560 modified carbon black, and no theoretical spectrum have been found. While compared with other relevant modification results, the spectrum obtained is basically consistent with the inferred results.

The significance of FTIR spectra is to prove the successful grafting of KH560 onto the surface of carbon black, so as to prove that further modification of carbon black to the surface of aluminum powder can be achieved theoretically.]

Comments 3: [In Fig.6, scale bar is not visible, please rescale it.]

Response 3: [Thank you for your suggestion. The scale bar in Fig. 6 has been modified (Page 8, line 301).]

Comments 4: [Al, O and C elemental XPS spectrum are need to add and discuss in revised manuscript.]

Response 4: [Thank you for your valuable advice. After the modification of SiO2 and carbon black, the amount of the Al element on the surface of aluminum powder is obviously reduced, and the peak value is weak, so that it is difficult to fit the Al peak well. In addition, the Si peak fitting is sufficient to confirm the modification success, so I personally think it is not necessary to carry out sub-peak fitting for Al, O and C.]

Comments 5: [what is relationship of H2 yield vs corrosive protective coatings? please specify clearly.]

Response 5: [Thank you for your suggestion. The stability of aluminum powder in water-borne coating system can be analyzed and obtained by the characterization of hydrogen evolution of aluminum powder. The smaller hydrogen yield means that the powder exhibits high stability under the water-borne coating, so a stable anti-corrosion coating can be made, but not the opposite. This is mentioned in the first paragraph of the part of “3.6. Hydrogen evolution behavior” (Page 12, line 405).]

Comments 6: [EIS spectra of the materials need to study in depth and discuss the details of EIS spectra in revised manuscript.]

Response 6:[Thank you for your suggestion. This paper fucuses the surface modification of aluminum powder, and concentrates on the storage stability of aluminum powder in water-borne system and the electrical conductivity of aluminum powder, so only the polarization resistance of the coating is preliminarily analyzed by polarization test, but the coating corrosion was not studied further. Therefore, EIS and other analyses were not carried out on the coating. In the future, we will further study the coating properties and improve our work.]

Comments 7: [for sake of competence and improve the readership of this article, authors refer and cite these articles in introduction part: RSC advances 14 (20), 14263-14277; Materials 2024, 17(1), 126; https://doi.org/10.3390/ma17010126; Alexandria Engineering Journal 59 (6), 4449-4462; Coatings 2021, 11(4), 453; https://doi.org/10.3390/coatings11040453]

Response 7: [Thank you for your suggestion. Relevant literature has been added to the paper according to your comments (Page 17, lines 598-612, literature 3, 5, 9, 10).]

Comments 8: [There are several typo and format errors, please revise.]

Response 8:[Thank you for your suggestion. The typo and format errors have been revised by a professional teacher. There are more modifications, please see the highlights in the manuscript.]

Round 2

Reviewer 1 Report

Comments and Suggestions for Authors

The authors have revised the previous manuscript following the reviewers' suggestions and comments appropiately. The reviewer therefore supports this revised manuscript for publication by this journal. 

Author Response

Thank you for your recognition of this work.

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