Ultrasound-Assisted Synthesis for the Control of Silver Nanoparticle Size: A Preliminary Study on the Influence of Pressure and pH
Round 1
Reviewer 1 Report
Comments and Suggestions for AuthorsThe topic of this paper is to explore the influence of pH and pressure on the sizes of silver nanoparticles, because the size and morphology are essential for applications, such as SPR. The experimental results show that pH and pressure have an important impact on the diameter of silver nanoparticles. However, in my opinion, this manuscript needs major revisions or Resubmit the paper after revision before it can be accepted for publication. Herein, my comments are as follows:
(1) In the title, “Preliminary Study on Pressure and pH control of the Size of Silver Nanoparticles: A Rapid and Cost-Effective Ultrasound Assisted Synthesis for further applications” , while “A Rapid and Cost-Effective Ultrasound Assisted Synthesis for further applications” should be deleted, because it is rarely mentioned in the text, and it has little to do with the research topic.
(2) In the “Introduction”, what progress has been made on the effects of pressure and pH on the sizes of silver nanoparticles, and what difficulties still need to be solved? How does this study solve this problem?
(3) In the “Results”, the resolution of the illustrations in Figure 4, Figure 5 and Figure 6 are too low to see clearly, and the high-resolution illustrations should be provided.
(4) In the “Conclusions”, the main conclusions of the paper are presented succinctly, rather than being heavily copied.
(5) The whole paper is not concise, verbose and illegible. This paper needs careful revision.
Comments on the Quality of English LanguageThe topic of this paper is to explore the influence of pH and pressure on the sizes of silver nanoparticles, because the size and morphology are essential for applications, such as SPR. The experimental results show that pH and pressure have an important impact on the diameter of silver nanoparticles. However, in my opinion, this manuscript needs major revisions or Resubmit the paper after revision before it can be accepted for publication. Herein, my comments are as follows:
(1) In the title, “Preliminary Study on Pressure and pH control of the Size of Silver Nanoparticles: A Rapid and Cost-Effective Ultrasound Assisted Synthesis for further applications” , while “A Rapid and Cost-Effective Ultrasound Assisted Synthesis for further applications” should be deleted, because it is rarely mentioned in the text, and it has little to do with the research topic.
(2) In the “Introduction”, what progress has been made on the effects of pressure and pH on the sizes of silver nanoparticles, and what difficulties still need to be solved? How does this study solve this problem?
(3) In the “Results”, the resolution of the illustrations in Figure 4, Figure 5 and Figure 6 are too low to see clearly, and the high-resolution illustrations should be provided.
(4) In the “Conclusions”, the main conclusions of the paper are presented succinctly, rather than being heavily copied.
(5) The whole paper is not concise, verbose and illegible. This paper needs careful revision.
Author Response
Please see attached the reply to your comments.
Author Response File: 
Author Response.pdf
Reviewer 2 Report
Comments and Suggestions for AuthorsThis article reports “Preliminary Study on Pressure and pH control of the Size of Silver Nanoparticles: A Rapid and Cost-Effective Ultrasound-Assisted Synthesis for further applications”. Although this study provides some detailed synthesis and analytical results, the reviewer believes the current research findings, data presentation, and discussion cannot meet the publication criteria of Condensed Matter. There are several concerns that should be addressed as listed herein:
- It is not clear where the paper is making a new context in the field of Ag NPs synthesis, problem orientation and claim of work should be further addressed.
- Authors should briefly explain how pressure and pH influence the size of the prepared silver nanoparticles and how this contributes to their potential applications.
- Reviewers are unable to find valuable insights based on the proposed research in the introduction section. The authors need to carefully revise the introduction.
- Authors should move the "Materials and Methods" section from Section 4 to Section 2
- In Figure 2C-D, the caption and the text inside the figure are completely different. The authors should revise carefully.
- The discussion of Figures 1 and 2 needs further improvement.
- The authors stated that the prepared Ag NPs have a spherical structure. However, the reviewers could not identify a uniform spherical structure, and the image quality needs improvement. The authors should revise the images accordingly.
- In Fig. 6A, the reported EDX analysis for Ag NPs shows numerous impurity elements. However, the reviewers found many impurities in the EDX results. The authors should provide an explanation for these impurities.
- In addition to above points, a thorough inspection is really required, because many typographical, grammatical errors or poor English are distributed in the manuscript, the manuscript should be carefully checked, and necessary corrections should be done.
Examples of poor English or grammatical errors are listed herein:
* Line 67-70…
* Line 110-118…
* Line 127-132…
* Sec 2.1…
* Sec 4.4 and etc…
Comments for author File: Comments.pdf
In addition to above points, a thorough inspection is really required, because many typographical, grammatical errors or poor English are distributed in the manuscript, the manuscript should be carefully checked, and necessary corrections should be done.
Examples of poor English or grammatical errors are listed herein:
* Line 67-70…
* Line 110-118…
* Line 127-132…
* Sec 2.1…
* Sec 4.4 and etc…
Author Response
Please see attached the reply to your comments.
Author Response File: Author Response.pdf
Reviewer 3 Report
Comments and Suggestions for AuthorsI recommend that this paper be accepted after major revision.
After carefully reviewing this work, I found that the manuscript has good strength and has shown interesting work with highly appreciated protocol. Still, it requires some major revisions, and the questions below are clarified:
1- EDX Results Interpretation
Analysis showed only 3% silver content; it was lower than you would expect (EDX). Authors state that this can be attributed to the matrix (for example, copper/aluminum from the grid) but this provides a lackluster explanation. You need to have a conversation about whether that incomplete reduction or even contamination is okay. Furthermore, this would increase transparency if it was made clear if the EDX data were normalized or quantified with background subtraction.
2- Pressure Treatment Rationale
There is no rationale for the selection of 1.75 MPa and 200°C for its pressure treatment. How do these parameters´ compares to other previous studies? Are they the best possible for nanoparticle development? This would help the section, a short literature comparison or initial optimization just like is done in the method section.
3- pH Effects and Buffer Interference
While the absence of these SPR peaks at pH 4 and 7 (Fig. 2 B) is explained by ionic strength contributions from buffers, the mechanism remains unexplored. Is citrate buffer (pH 4) chelating Ag⁺ ions & preventing the nucleation, for example? A more detailed explanation of pH specific interactions (e.g., protonation of citrate) would be useful.
4- Comparison with Literature
Although references have been cited, direct comparisons between similar studies (e.g., ultrasound-assisted synthesis under different pH/pressure) are few. Placing the specifics on how this work takes the field forward (e.g., decreased particle sizes compared to that in earlier methods) would clearly illustrate how novel this work is.
5- Minor Comments Figures and Tables
Figures mentioned in the text (E.g.: Figures 2, 3, 5) are not shown in the data. Include high-resolution images with clear labels (e.g. scale bars in STEM images). In Table 1, please specify if "NPs size" means hydrodynamic diameter or size as measured under TEM?
6- Language and Typos
There are in fact some typographical errors: “synthetized” → “synthesized” (throughout), inconsistent use of decimal commas (like in “pH 4,0” vs. “pH 7.0”), and abuse of hyphens (like in “cost effective” → “cost-effective”). It is advised that you proofread this document extensively.
7- Stability Over Time
The 28-day stability data are a strong point. In addition, you may try adding the zeta potential measurements to relate stability with respect to the surface charge.
8- Mechanistic Insights
Explain how nucleation/growth is controlled precisely by ultrasound energy in method 1 as compared to method 2. Does cavitation cause reduced aggregation?
Comments for author File: Comments.pdf
Author Response
Please see attached the reply to your comments.
Author Response File: Author Response.pdf
Round 2
Reviewer 2 Report
Comments and Suggestions for AuthorsI agree to published this paper to Condensed Matter.
Reviewer 3 Report
Comments and Suggestions for AuthorsThe authors have addressed my comments and made significant improvements compared to the previous version. I recommend acceptance.
