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Article
Peer-Review Record

Cold Plasma Deposition of Polymeric Nanoprotrusion, Nanoparticles, and Nanofilm Structures on a Slide Glass Surface

Processes 2021, 9(1), 99; https://doi.org/10.3390/pr9010099
by Sun-Woo Yi 1, In-Keun Yu 2, Woon-Jung Kim 3,* and Seong-Ho Choi 1,3,*
Reviewer 1:
Reviewer 2: Anonymous
Processes 2021, 9(1), 99; https://doi.org/10.3390/pr9010099
Submission received: 28 November 2020 / Revised: 26 December 2020 / Accepted: 4 January 2021 / Published: 5 January 2021
(This article belongs to the Special Issue Plasmochemical Processes and Their Technological Applications)

Round 1

Reviewer 1 Report

This paper describes a cold plasma deposition method to form polyvinyl coatings on glass slides. The experiments are adequately described and the results are clearly presented.

However, I think the authors should clarify some claims before the paper is published:

  1. The sentence in line 93, "due to the lower transmittance of the plasma-coated poly(TFMA/MMA)", is redundant with the previous one. It is quite obvious that transmittance decreases because a coating was deposited, there is no need to state it. I suggest deleting this sentence.
  2. All images reporting contact angle measurements display unusual drop shapes, namely drops look deformed vertically. I think the authors should make sure that drop profiles are not deformed.
  3. Throughout the text (e.g. line 146) the authors claim that "no dipole moments are present due to symmetric polarity" of the monomers. It might be true, however I suggest to add calculations of the actual dipole moments of the monomers to justify this claim.
  4. In line 155, the authors state that "the transmittance of the poly(TSMA-co-MMA)-coated slide was less than that of the poly(TFMA-co-MMA)-coated slide 157 because of the Si group". First, "Si group" is not accurate, as it is a Si(CH3)3 group. Second, the authors should specify why such group leads to lower transmittance.
  5. In line 189, the authors state that "poly(TSMA-co-MMA) formed a plate film with air bubbles". Does "plate" mean "flat"? The micrographs in Fig.11 do not show a flat film at all, as protrusions ar clearly visible. I suggest to reformulate this sentence.

Author Response

1. The sentence in line 93, "due to the lower transmittance of the plasma-coated poly(TFMA/MMA)", is redundant with the previous one. It is quite obvious that transmittance decreases because a coating was deposited, there is no need to state it. I suggest deleting this sentence.

- Response : Thank you for your attentive comment. According to your comment, we deleted as following sentence: while the transmittance decreased after plasma polymerization of feed solution with TFMA/MMA due to the lower transmittance of the plasma-coated poly(TFMA/MMA).

2. All images reporting contact angle measurements display unusual drop shapes, namely drops look deformed vertically. I think the authors should make sure that drop profiles are not deformed.

- Response : Thank you for your comment. We fixed the figures of contact angle.

3. Throughout the text (e.g. line 146) the authors claim that "no dipole moments are present due to symmetric polarity" of the monomers. It might be true, however I suggest to add calculations of the actual dipole moments of the monomers to justify this claim.

- Response : We agreed your comments. We removed as following sentence: no dipole moments are present due to symmetric polarity

4. In line 155, the authors state that "the transmittance of the poly(TSMA-co-MMA)-coated slide was less than that of the poly(TFMA-co-MMA)-coated slide 157 because of the Si group". First, "Si group" is not accurate, as it is a Si(CH3)3 group. Second, the authors should specify why such group leads to lower transmittance.

- Response : According to your comment, we revised as follows: because of the Si(CH3) group, which is inorganic element with lower transmittance

5. In line 189, the authors state that "poly(TSMA-co-MMA) formed a plate film with air bubbles". Does "plate" mean "flat"? The micrographs in Fig.11 do not show a flat film at all, as protrusions ar clearly visible. I suggest to reformulate this sentence.

- Response : Thank you for your comment: According to your comments, We revised as follows: When a large amount of MMA was added to the feed solution, the coated poly(TSMA-co-MMA) formed a flat film, as shown in No. 5 in Fig. 9, due to the poly(MMA).

Reviewer 2 Report

The authors must present details of their cold plasma deposition system, since people cannot evaluate or reproduce their results based on the superficial description on page 2, lines 66-71. 

The authors must provide evidence to support their conceptual picture shown in Fig. 13.

 

Author Response

1.The authors must present details of their cold plasma deposition system, since people cannot evaluate or reproduce their results based on the superficial description on page 2, lines 66-71. 

- Response : Thank you for your comments. According to your comment, we added the reference [12,13], which is reported before our laboratory. Line 204, 264~268.

2. The authors must provide evidence to support their conceptual picture shown in Fig. 13.

- Response : Thank you for your comment. In a previous paper [12,13], we reported the mechanism of the polymerization via diverse data. So, we also added the reference [12,13]. Line 204, 264~268.

Round 2

Reviewer 1 Report

The authors responded to all my questions, however I think some answers were not on point:

  • Line 144 states "We expected that the specimen would be superhydrophobic due to a lack of dipole moments from the sum of symmetric polarity". I think hydrophobicity is rather expected because of -CH3 groups, which are known for their capacity to induce hydrophobicity. I suggest rephrasing.
  • In Line 153 "Si(CH3) group" is mentioned, but is rather a Si(CH3)3 group. Moreover, the authors should add at least one reference that justifies the claim that this group leads to reduced transmittance.
  • Lines 185-187 are very confusing. Fig.9 is supposed to display images from sample No.1 and 2, while Fig.11 is related to sample No.5. Moreover, the film in Fig.11 does not seem flat at all, it rather looks nanostructured. I suggest adding roughness measurements to compare samples No.1 and 2 with sample No.5 to support the claim.

Author Response

1. Line 144 states "We expected that the specimen would be superhydrophobic due to a lack of dipole moments from the sum of symmetric polarity". I think hydrophobicity is rather expected because of -CH3 groups, which are known for their capacity to induce hydrophobicity. I suggest rephrasing.

- Response: Thank you for your advice. We accepted your comment. We added the as following sentence. We think hydrophobicity is rather expected because of -CH3 groups, which are known for their capacity to induce hydrophobicity(148~149 line)

2. In Line 153 "Si(CH3) group" is mentioned, but is rather a Si(CH3)3 group. Moreover, the authors should add at least one reference that justifies the claim that this group leads to reduced transmittance.

- Response: Thank you for good suggestion. According to your advice, we revised and add the reference [13] to revised manuscript(158, 269, 270 line).

3. Lines 185-187 are very confusing. Fig.9 is supposed to display images from sample No.1 and 2, while Fig.11 is related to sample No.5. Moreover, the film in Fig.11 does not seem flat at all, it rather looks nanostructured. I suggest adding roughness measurements to compare samples No.1 and 2 with sample No.5 to support the claim.

- Response: Thank you for your comments. We agreed your comment for No. 5 with nanostructure. We claimed the flat form structure of the samples coated with poly(MMA) of 100%. We have very difficult situation, now, to measure the roughness through AFM equipment because of CORONA-19 pandemic.

Reviewer 2 Report

The two references, 12 and 13, do not provide sufficient details of their cold plasma deposition system for readers to evaluate or reproduce their results. 

Author Response

The two references, 12 and 13, do not provide sufficient details of their cold plasma deposition system for readers to evaluate or reproduce their results. 

- Response: We described the suggested mechanism (Fig, 13) in 4. Discussion part, not 3. Results. According to 3. Result and the previous papers, we described the suggested mechanism in 4. Discussion part. In our opinion, the suggested mechanism is no problem because of Discussion part.

Round 3

Reviewer 2 Report

The authors still do not provide the details of their cold plasma deposition system. The details, such as the plasma generator (homemade or purchased (if the latter, please provide the manufacturer)), energy density, temperature of the plasma, and any relevant info to help readers to build a similar system, should be disclosed.

Author Response

The authors still do not provide the details of their cold plasma deposition system. The details, such as the plasma generator (homemade or purchased (if the latter, please provide the manufacturer)), energy density, temperature of the plasma, and any relevant info to help readers to build a similar system, should be disclosed.

Response : Thank you for your comments. According to your comments, we give the detailed plasma equipment. The plasma equipment was directly obtained from Applied Plasma Inc. (model 3D+iCVC SINGLE) at Gumi City, Korea. The plasma equipment have voltage with input 220V and output 15 KV rms, amphare with input 5A and output 70 mA, frequency with input 60 Hz and output 30~40 KHz, phase with input single and output single, and air pressure with input 0.5Mpa and output 0.025 Mpa, respectively.(line 68~73)

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