Laser Processing of Liquid Feedstock Plasma-Sprayed Lithium Titanium Oxide Solid-State-Battery Electrode

Round 1

Reviewer 1 Report

Comments and Suggestions for Authors

Full Title: Laser processing of liquid feedstock plasma-sprayed Lithium 2 Titanium Oxide (LTO) solid-state-battery electrode

In the present work, the effects of laser beam interaction with a liquid feedstock plasma-sprayed ceramic solid-state-battery (SSB) material coating were studied. Lithium Titanium Oxide (LTO) in the form of aqueous suspension consisting of submicron powder particles was for the first-time plasma-sprayed using the high-power axial III plasma torch on an aluminum sub- strate. The abstract need covers some results that mentioned in paper, to be better. The introduction is need to be more comprehensive and the experimental work is need discussion. Some comments could be summarized as follows:

 

1-     In the abstract should be rewritten , you should to refer on the induced changes of properties with some data.

2-     You should to refer in the introduction part, what is the reason for choosing plasma-sprayed Lithium 2 Titanium Oxide (LTO) (it need some novelty(?

3-     The objectives are not clear – You should to mention the objective and the novelty of the work in the last paragraph of the introduction part?

4-     Why author has with 20 wt. % solid LTO powder and 1 wt.% of 1-Methyl-2-pyrrolidinone 118 (NMP) (Sigma-Aldrich) as an additive.? Give the practical reason for selecting these values?

5-     Some mistake in the manuscript and reparation (such as you Equation 1. Is repeated). You should revise the full manuscript carefully.

6-     The rough surface is mostly important for discuss the behavior presence of hilly areas. The authors should discuss it with respect to the modifications to the surface. Please discuss the reasons for the change?

7-     Results are interesting, but should to be more discussion and comparison with other works?

8-     In SEM, need more discussion to refer for the reasons of no significant appearance differences between the laser post-processed zone and the non-laser processed area?

9-     In result and discussion part, in Elemental distribution, you must to discuss the successful fabrications of the samples by refer to the percentage of the atoms in the text, need more discussion?

10- How to measure the sample thickness?

11- Conclusions, should to be more directed toward the applications of these samples for solid-state-battery electrode Applications?

12- You must to update the refs, to be new and related of the work. 

 

Comments for author File: Comments.pdf

Author Response

Dear reviewer,

The authors appreciate the insightful feedback from the reviewer. Please find the detailed responses in the attached file.

BR,

Arman Hasani

Author Response File: Author Response.pdf

Reviewer 2 Report

Comments and Suggestions for Authors

The research article entitled “Laser processing of liquid feedstock plasma-sprayed Lithium Titanium Oxide (LTO) solid-state-battery electrode” is gone through carefully. This manuscript presents an insightful study on the influence of laser processing on the surface morphology and chemical composition of plasma-sprayed LTO coatings, which is a critical aspect in solid-state battery technology.

The authors have meticulously executed the experimental work, providing detailed insights into the effects of varying laser processing parameters. The comprehensive utilization of SEM imaging and elemental mapping significantly enhances the clarity and understanding of the study's outcomes. Furthermore, the manuscript is well-structured, with a clear and concise presentation.

 

However, I recommend a few areas for improvement:

 

1. The manuscript notes no significant appearance differences between the laser-processed zone and the non-laser processed area yet mentions an observable improvement in surface smoothness in the laser-processed region​​. This statement appears contradictory and needs clarification. A more detailed explanation of the criteria used to assess 'significant appearance differences' and how the improved surface smoothness was quantified would be beneficial.

 

2. The manuscript discusses improved coating properties such as decreased surface roughness due to laser post-processing​​. It would be advantageous to include more quantitative data or comparative analysis to substantiate these improvements. This could include specific measurements of surface roughness before and after laser processing or comparisons with other post-processing techniques.

 

3. The study discusses the chemical composition differences between as-sprayed, laser-processed, and non-laser processed zones​​. While it is noted that there are no significant differences in titanium and carbon content, and an increase in oxygen content due to oxidation, the manuscript would benefit from a more in-depth analysis of these findings. Specifically, a more detailed discussion on the implications of these elemental changes on the performance and durability of the LTO coatings would be valuable.

 

4. It is noted that Li could not be detected as it is beyond the detection limit of EDS. This is a significant limitation, considering the importance of lithium in the context of lithium titanium oxide coatings for solid-state batteries. The manuscript should address this limitation more thoroughly, discussing potential alternative methods for lithium detection or quantification, and the impact of this limitation on the overall conclusions of the study.

Author Response

Dear reviewer,

The authors appreciate the insightful feedback from the reviewer. Please find the detailed responses in the attached file.

BR,

Arman Hasani

Author Response File: Author Response.pdf

Reviewer 3 Report

Comments and Suggestions for Authors

The authors presented a method to modify SSB electrodes using a laser. However, due to the lack of completeness, repeatability, and refinement of experiments, they are unable to prove the usefulness of this method. So it doesn't provide a strong advantage over other methods. The followings need to be revised.

 

1. The authors are calculating the energy input by dividing the energy by the area. Is this a correct assumption, and is there no difference in intensity between the center and the edges?

2. There are a lot of mistakes in the expression of equations throughout the paper. Use italics and roman for their respective purposes. And the authors need to use symbols in their equations and explain the meaning of those symbols in sentences. Also, the formula contains units in a weird form.

3. Please provide the information of the equipment and materials in a generic way. Include the name, model, and country of origin.

4. How did the authors calculate the error in Figure 3? Did they do multiple experiments? Or was it derived from the results in Figure 1? Moreover, lines 2,4 are severely curved.

5. Figure 4 is hard to recognize. The authors need to include both the center and edge areas of the laser.

6. In Figures 4 and 6, as the roughness gets smaller, shouldn't the error also get smaller? But regardless of the roughness, the error seems to be about the same size. As illustrated by Figure 5, the error should be small. What do you think?

7. In Table 6, the authors used EDS to estimate elemental composition. However, I think EDS is not accurate enough for such an analysis. The authors need to use other methods to enhance this analysis.

8. The authors show the results of their experiments on a single wafer. It is necessary to repeat the experiment several times to increase the reliability of the data.

9. The authors are only focusing on the shape of the surface. However, they need to show that SSB made this way have higher performance.

Comments on the Quality of English Language

The English language is no problem, but it lacks the formatting of engineering paper, such as equations.

Author Response

Dear reviewer,

The authors appreciate the insightful feedback from the reviewer. Please find the detailed responses in the attached file.

BR,

Arman Hasani

Author Response File: Author Response.pdf

Round 2

Reviewer 2 Report

Comments and Suggestions for Authors

I have reviewed the revised manuscript titled "Laser processing of liquid feedstock plasma-sprayed Lithium Titanium Oxide (LTO) solid-state-battery electrode". The improvements made in response to previous comments are commendable and have enhanced the quality of the manuscript substantially. Therefore, I recommend accepting the manuscript for publication.

Author Response

The authors appreciate your positive feedback.

Author Response File: Author Response.pdf

Reviewer 3 Report

Comments and Suggestions for Authors

The authors have revised the manuscript, but it is still incomplete. Reviewer suggestions are rarely considered, and sometimes even simple text edits are not made. I would like to reject the publication due to the lack of methodological incompleteness and lack of academic significance. The authors suggested to change followings and apply to another journal.
 

1. To improve the reliability of experiment, authors need to conduct multiple experiments. Conducting an experiment once and then picking clear spots to analyze is not the right way to experiment.

2. These insufficient experiments cause the authors to misinterpret their results. So, as another reviewer pointed out, the author's claims seem to contradict each other.

3. It also lacks scientific novelty.

Comments on the Quality of English Language

The English language expression is no problem, but it lacks the formatting of an engineering paper, such as equations.

Author Response

The authors appreciate your comments.

Author Response File: Author Response.pdf