Simple Approach to the Fabrication of Lanthanum Orthoniobates and Nanocomposites with Ni, Cu, and Co Metal Nanoparticles Using Supercritical Isopropanol
, Konstantin Valeev 2, Nikita Eremeev 2, Ekaterina Sadovskaya 2, Tamara Krieger 2, Artem Ulihin 3, Arina Uhina 3, Bakytgul Massalimova 1, Mikhail Simonov 2 and Vladislav Sadykov 2
Round 1
Reviewer 1 Report
The reviewed article entitled “Simple approach to the fabrication of lanthanum orthoniobates and nanocomposites with Ni, Cu, Co metal nanoparticles using supercritical isopropanol” reports interesting data on the preparation and characterization of cermet composites based on Ni-alloys and LaNbO4-oxides. The provided research utilizes a number of complementary techniques to reveal composition/structure/properties regulations. However, the following comments need to be addressed before the publication of this article.
â–º The ENG syntax and grammar are insufficient; please provide proofreading by a native speaker to improve overall language quality
â–º Introduction. Please indicate the reasons for the preparation of NiCu/niobate and NiCo/niobate composite materials.
â–º Materials and Methods. A %-purity of each compound should be provided, since “pure for analysis grade” is unclear for me.
â–º The temperature treatments should be detailed. What does 500–1000 °C for 4 h or 700–1000 °C for 6 h mean?
â–º Figure 2a. Additional particles are visible over the surface of the LCNb ceramics. Is this an impurity? Please confirm your response by experimental data.
â–º Figure 10 should be supplied with the EDX analysis to show which grains belong to the LCNb or metallic alloy phases.
â–º Fig. 11b. There is the incorrect symbol (s instead of σ).
â–º I recommend to include and discuss some of the following recent work for improving the novelty and relevance of your work:
https://doi.org/10.1016/j.jallcom.2020.157532
https://doi.org/10.1002/pssa.202100748
https://doi.org/10.3390/ma15062267
https://doi.org/10.3390/molecules26113179
https://doi.org/10.7566/JPSJ.91.091010
https://doi.org/10.1007/s10854-022-08093-0
https://doi.org/10.1016/j.snb.2021.130981
https://doi.org/10.1016/j.electacta.2021.139495
https://doi.org/10.3390/met11121892
https://doi.org/10.1016/j.cej.2021.128977
Author Response
Point 1: The ENG syntax and grammar are insufficient; please provide proofreading by a native speaker to improve overall language quality
Response 1: Done.
Point 2: Please indicate the reasons for the preparation of NiCu/niobate and NiCo/niobate composite materials.
Response 2: To create highly efficient proton-conducting membranes, materials should be used with a set of characteristics, such as stability in various media (CO2, H2O), high mechanical strength, and, of course, high conductivity. It is not always possible for individual components to meet these requirements, so approaches such as the use of composites will help to solve this problem. The introduction of a metal component into the composite provides high electronic conductivity which is crucial to avoid hydrogen permeation limiting by coupled electron-proton transport across the membrane.
Point 3: Materials and Methods. A %-purity of each compound should be provided, since “pure for analysis grade” is unclear for me.
Response 3: Corrected.
Point 4: The temperature treatments should be detailed. What does 500–1000 °C for 4 h or 700–1000 °C for 6 h mean?
Response 4: Corrected in text.
Point 5: Figure 2a. Additional particles are visible over the surface of the LCNb ceramics. Is this an impurity? Please confirm your response by experimental data.
Response 5: Yes, additional particles are visible over the surface of the Lb ceramics, but it isn't an impurity. During experiment ( shooting) the surface is recharged.
Point 6: Figure 10 should be supplied with the EDX analysis to show which grains belong to the LCNb or metallic alloy phases.
Response 6: Unfortunately, at the moment we cannot carry out the analysis, but in the future works we will definitely realize this study. In any case grains observed in Fig. 10 are in the range of 0.5-3 microns, while in Fig. 7 sizes of areas corresponding to each element aggregation are less than 0.1 microns. This implies that all grains observed in Fig. 10 are comprised of nanocomposites, which provides their high mixed protonic-electronic conductivity and hydrogen permeation due to developed interfaces.
Point 7: Fig. 11b. There is the incorrect symbol (s instead of σ).
Response 7: Corrected.
Point 8: I recommend to include and discuss some of the following recent work for improving the novelty and relevance of your work:
https://doi.org/10.1016/j.jallcom.2020.157532
https://doi.org/10.1002/pssa.202100748
https://doi.org/10.3390/ma15062267
https://doi.org/10.3390/molecules26113179
https://doi.org/10.7566/JPSJ.91.091010
https://doi.org/10.1007/s10854-022-08093-0
https://doi.org/10.1016/j.snb.2021.130981
https://doi.org/10.1016/j.electacta.2021.139495
https://doi.org/10.3390/met11121892
https://doi.org/10.1016/j.cej.2021.128977
Response 8: Thank you very much for the list of contemporary literature, links are inserted into the text.
Reviewer 2 Report
The article "Simple approach to the fabrication of lanthanum orthoniobates and nanocomposites with Ni, Cu, Co metal nanoparticles using supercritical isopropanol" is a well written contribution reporting the study of NiCu and NiCo nanoparticles and rare-earth orthoniobates powders synthesized by a supercritical alcohol fluid technology. I only have a few minor points:
1. Page 2, line 91, the formula CoxOy and Bi2O3 should have the numbers/variables subscript.
2. Page 6, line 224, in the formula Co3O4, the numbers should be subscript.
3. Page 10, line 289, the symbol of degrees calcium is not correct. Please use the same that is in line 298. Also, please check for other similar situations in the entire manuscript.
4. Figure 11 axis, the decimal separator has commas instead of dots. Also in Fig 11 b, the Greek symbol for conductivity is missing.
Author Response
Point 1: line 91, the formula CoxOy and Bi2O3 should have the numbers/variables subscript.
Response 1: Corrected.
Point 2: Page 6, line 224, in the formula Co3O4, the numbers should be subscript.
Response 2: Corrected.
Point 3: Page 10, line 289, the symbol of degrees calcium is not correct. Please use the same that is in line 298. Also, please check for other similar situations in the entire manuscript.
Response 3: Corrected
Point 4: Figure 11 axis, the decimal separator has commas instead of dots. Also in Fig 11 b, the Greek symbol for conductivity is missing.
Response 4: Corrected.
Round 2
Reviewer 1 Report
This response should be properly presented in the text instead of 'response to the reviewer's comments' only
Point 2: Please indicate the reasons for the preparation of NiCu/niobate and NiCo/niobate composite materials.
Response 2: To create highly efficient proton-conducting membranes, materials should be used with a set of characteristics, such as stability in various media (CO2, H2O), high mechanical strength, and, of course, high conductivity. It is not always possible for individual components to meet these requirements, so approaches such as the use of composites will help to solve this problem. The introduction of a metal component into the composite provides high electronic conductivity which is crucial to avoid hydrogen permeation limiting by coupled electron-proton transport across the membrane.
Author Response
Many thanks for the detailed and thorough review of our article. The description of the reasons for the preparation of NiCu/niobate and NiCo/niobate composite materials is inserted in the text of the article.
Reviewer 2 Report
The current version is now ready for publication.
Author Response
Thank you so much for reviewing our article!Round 3
Reviewer 1 Report
The authors have addressed all my comments. Therefore, this article can be accepted for publication as it is.
