Structural, Morphological and Optical Properties of Nanostructured ZrO2 Films Obtained by an Electrochemical Process at Different Deposition Temperatures
Round 1
Reviewer 1 Report
Konstantin Lovchinov et. al, elaborated the paper with the title: “Structural, Morphological and Optical Properties of Nanostructured ZrO2 Films Obtained by an Electrochemical Process at Different Deposition Temperatures”, where comprehensive studies regarding metal oxide nanostructured materials are presented. The deposition method applied, namely the electrochemical process has the advantage for its low operating cost and its simple experimental configuration, making any relating studies and results very attractive as providing a possible knowledge transfer to the industry. I find the article as being well structured, well written and assisted by relevant data and I recommend it for publication after authors implement minor changes as mentioned below:
- Authors should reconsider double checking the format and different mistakes in text (ex. In title “Zro2”…); Also, include department into the affiliation, authors should review the publishing guidelines;
- Since keywords have generally a impact in making the paper more viewable, authors could consider identifying and including additional keywords;
- Please add manufacturer of all implied instruments and materials, as mentioned in the publishing guidelines; Also, add concentrations / purity for used materials. Therefore, authors should further add information to “Methods and materials” section;
- What is the Z resolution of the Zeta 20 3D optical profilometer?
- Figure captions should be more explicative; thus, reader should understand the presented results without referring to text;
- Only as a suggestion, in general, the theory and equations could be mentioned in section 2 “materials and methods”; Also, a suggestion relating the text font/color, authors should avoid using red color (in tables), since it could express unintentionally a corrupted data instead of point out the high calculation errors;
- In table 2, please add the missing information on the temperature (first column). Please mention the purpose of using the blue color.
- Improve the quality of figures found in fig. 3., the scale is not viewable. Make the figures larger;
- What software was used for the determination of RMS values; Does here reported results on RMS could also be referred to other papers?
- Please increase the contrast of the scale in the SEM images. Authors could further post-process the images in order to address the density of particles or voids (as line profiles or mappings overviewing the gray level variations), thus adding more value to the statement “is an evident increase in the size of the grains located on the surface…”; Could the SEM images be followed by EDX measurements? Please discuss;
- The following phrase: “The shape of the grains of which the layers are composed is relatively spherical and regular, as the layer with the closest to spherical shape formations..” is heavily relying on ones visual inspection and not followed theoretical premise; When it comes to sphericity, authors should qualify it by precise use of equations, further classifying a grain as elongated, regular etc.
- Figure 5, please increase the contrast at a optimal level (as seen in figure 6);
- Add ICDD cards associated to the XRD results;
- When it comes to interpreting the transmission, diffuse transmission and haze ratio spectra, authors should also add reference to results described by other research groups;
- In the conclusion section, authors should point out the answer to the following questions: What is the novelty of the presented work? How the results compares with other deposition methods? Even if generally states, it should have an impact on the readers.
Author Response
Thank you very much for your positive comments and helpful remarks.
Author Response File: 
Author Response.docx
Reviewer 2 Report
The manuscript by Lovchinov et al. described the structural and optical properties of nanostructured ZrO2 films deposited at different temperatures. The work provides data that might be potential use for readers to reference to. However, one of the major issues of this manuscript is a lack of sufficient supporting data for conclusions made. Data is missing or disagree with the conclusions in some cases. The authors need to address these issues before the manuscript is considered for publication.
1. The temperature range referred to in the abstract and in the context is different. Line 13, 50-80°C; line 67, 60-80°C. The solution concentration is also different in line 15 and in line 66. Please be consistent.
2. The deposition temperatures referred to this this work, is it the solution temperature or the substrate temperature? This information is important to be included in the manuscript.
3. In section 2, deposition and characterizations of ZrO2 films should be described in separate paragraphs.
4. Line 122. Figure 3c is for film deposited at 70°C, not 65°C. It’s hard to conclude from Figure 3 that the film deposited at 65°C has the highest inhomogeneity. The explanation for the high surface roughness due to different velocity of ions in line 124-127 need to be supported by data or references. Otherwise it’s just simply an invalid argument.
5. Similar for conclusions made in line 143-146, supporting evidence is missing.
6. Figure 4. There’s no scale bar in the figures to determine the size of the grains.
7. Definition of haze ratio used in this work is missing.
8. For data shown in Figure 5 and 6, spectra collected from SnO2 substrate is missing for comparison.
9. Line 157. Thickness for films deposited at different temperatures need to be measured and shown here as supporting evidence.
10. Throughout the manuscript, there exits many places where ‘zirconium’ was used to refer to ‘zirconia’, such as those in line 149 and line 194.
Author Response
Thank you very much for your positive comments and helpful remarks.
Author Response File: Author Response.docx
Reviewer 3 Report
The authors have presented a paper entitled "Structural, Morphological and Optical Properties of Nanostructured ZrO2 Films Obtained by an Electrochemical Process at Different Deposition Temperatures"
The authors described a ZrO2 electrochemically growth on top of a SnO2 covered glass at different temperatures (60º, 65º, 70º, 75º & 80º). All samples including the reference were analyzed by means of XRD, profilometry, SEM and UV-Vis-NIR.
I have several problems with the paper, some of the images are really poor quality, specially those from the profilometer. But , the main concern is that there is basically no discussion of why the results are as the are and only is everything associated to eh grain size , but no real deep understanding is developed during the paper. Thus, I do believe that at least in the present form this paper does not have the quality and does not contribute greatly to the field.
Author Response
Thank you very much for the helpful remarks.
Author Response File: Author Response.docx
Round 2
Reviewer 2 Report
text and format editing is needed
Author Response
Thank you for the positive assessment of our work
Author Response File: Author Response.docx
Reviewer 3 Report
The authors have made several upgrades to the manuscript and I do believe they have also enhanced the quality overall the information.
Therefore, I believe this time can be accepted just with a final english revision. With special emphasis in the new optical discussion paragraphs. I do believe the style can be improved.
Author Response
Thank you for the positive assessment of our work.
Author Response File: Author Response.docx
