Particle Formation Mechanism of TiCl₄ Hydrolysis to Prepare Nano TiO₂

Round 1

Reviewer 1 Report

Comments and Suggestions for Authors

This is a review for applsci-2705267: “Particle size regulation of TiCl4 hydrolysis to prepare nano TiO2 by Qianjun et al.

The article can be accepted with major modifications after addressing all the following comments very carefully.   

Comments

1. The introduction is too short. It should be extended.  

2.  Line 62: The equation of reaction is better to be on a separate line.  

3. Line 243: there is a maximum grain count of 102.2meshes per cubic

                      there is a maximum grain count of 102.2 meshes per cubic, add a space before meshes.

4. line 246: the D₅₀ is 0.19nm,      →  the D₅₀ is 0.19 nm, add a space before nm. Please check all similar cases.

5. Figure 11: The figure parts a and b need to be drawn on top of each other for clarity. Not on the side. Mass fraction ⁓f(D₅₀-T)  → Mass fraction ⁓ f (D₅₀-T) , add a space before and after f.

6. Before 3. Results and discussion part, the authors can mention something about the experimental part, and they can then discuss their results in the Results and Discussion part.

7. Compare your method with the experimental methods of SEM or TEM that prove the existence of produced nano-TiO₂.

8. The conclusions part is very general. It needs rewriting. It should contain some numbers, figures, concentrations and so on. Same applies to the abstract.

9. Make figures better separated. E.g. fig 3.

10. What is the accuracy of the method used?

11. There is no reference for the AspenPlus software. Where did you get it from? What version? Also input and output files need explanation.

12. The number of references should increase as a result of adding more literature and software usage explanation.

Comments on the Quality of English Language

Improve the English and structure

Author Response

Thank you for providing us with valuable suggestions. We have made timely modifications to this article and highlighted the modifications. We look forward to your reply again. Thank you.

Author Response File: Author Response.pdf

Reviewer 2 Report

Comments and Suggestions for Authors

 

Title: Particle size regulation of TiCl4 hydrolysis to prepare nano TiO₂

The impact of reaction time, temperature, water addition, pH value and ethanol content, on the crystal nucleation rate and particle size distribution (PSD) of TiO₂ in a water/water system ethanol was quantified. They report that T=300K, the formation of TiO2 crystal nuclei occurs mainly during the first 300 seconds. Also, they confirm that the quantity of water introduced is too low or too high, it influences the number of crystal nuclei and the size of the particles. Also, they confirm that under neutral pH conditions, the formation of crystal nuclei reaches its maximum, while the particle size decreases after growth.

In this paper the authors used Aspen chemical process simulation software. They integrated homogeneous nucleation theory and growth kinetics equations, to study the particle formation mechanism of TiCl4 hydrolysis in nanoscale TiO₂ synthesis.

 

The authors have to improve Figures 3, 5, 7, 9 and 11. Also, they should show the novelty of this work.

Comments on the Quality of English Language

In conclusion, this paper is important but it nneds minor revision. 

 

Author Response

Thank you for providing us with valuable suggestions. We have made timely modifications to this article and highlighted the modifications. We look forward to your reply again. Thank you.

Author Response File: Author Response.pdf

Reviewer 3 Report

Comments and Suggestions for Authors

The review report

The manuscript title: Particle size regulation of TiCl4 hydrolysis to prepare nano TiO₂.

In this paper, the authors used Aspen Plus software, to study the formation mechanism of TiCl₄ hydrolysis particles in TiO₂ nanoparticle synthesis. Aspen Plus software was used to simulate and measure the effects of different factors including reaction time, temperature, water addition, pH value and ethanol content on the crystal nucleation rate and TiO₂ particle size distribution (PSD) within the water/ethanol system. The results obtained showed that at ambient temperature, the nucleation of TiO₂ crystals occurs within the first 300 s, and then they move to the growth phase. The authors show that if the amount of water input is either too low or too high, it leads to a decrease in the number of crystalline nuclei formed and an increase in particle size. The authors claim to have found that under neutral pH conditions, the formation of crystal nuclei reaches a maximum, while a decrease in particle size is observed in the post-growth stage. Ultimately, the authors predicted that adding a small amount of ethanol stimulates the formation and growth of crystal nuclei, and that excessive ethanol content could have an inhibitory effect.

 

The authors used a few recent references (12 references), some of which are directly relevant to the topic of their manuscript. The manuscript has been prepared fairly adequately. The conclusions presented are consistent with the evidence and arguments presented, and address the main question raised.

 

Despite the importance of the topic addressed in this manuscript, it cannot be accepted for publication unless the following notes are taken into account:

 

1- All keywords must start with a capital letter.

2- The results should be enriched by comparisons with previous work.

3- The number of references must be increased and the size of the introduction must be increased.

4- The conclusion must be enriched by including a brief description of the research in addition to a narration of the results obtained.

5- The unique results obtained should be highlighted, especially in the abstract and conclusion.

 

Author Response

Thank you for providing us with valuable suggestions. We have made timely modifications to this article and highlighted the modifications. We look forward to your reply again. Thank you.

Author Response File: Author Response.pdf

Reviewer 4 Report

Comments and Suggestions for Authors

The document “Particle size regulation of TiCl4 hydrolysis to prepare nano TiO2” focused on the study of TiO2 growth by using Aspen Plus software.

After carefully reading the manuscript it was concluded that is more like a technical report that presents plots and graphs regarding the Aspen simulation. Only a small section of experimental validation was added and was not further discussed. Because Applied Science is a recognized journal with an impact factor of 2.7, the summited manuscript lacks the merit to be published in this Journal.

Author Response

Thank you for providing us with valuable suggestions. We have made timely modifications to this article and highlighted the modifications. We look forward to your reply again. Thank you.

Author Response File: Author Response.pdf

Round 2

Reviewer 1 Report

Comments and Suggestions for Authors

Authors did not provide a detailed coverletter for the changes they have made.

Introduction and references need more elaboration.

Conclusions are still weak.

Details of software and calculations are still not clear.

 

Comments on the Quality of English Language

OK

Author Response

Thank you for your valuable suggestions, here is the manuscript again revised with the cover letter.

Author Response File: Author Response.pdf

Reviewer 3 Report

Comments and Suggestions for Authors

The authors have completed the required revisions, so I suggest accepting the article for publication.

Author Response

Thank you for Your Hard Review, thank you

Reviewer 4 Report

Comments and Suggestions for Authors

After carefully checking the summited manuscript entitled "A kinetic model for the preparation of nano TiO2 by hydrolysis of TiCl4" its seems that the author forgets to send the rebuttal for the first round. Unfortunately, I can't make a review based only on the manuscript.

 

Author Response

Thank you for your valuable suggestions, here is the manuscript again revised with the cover letter.

Author Response File: Author Response.pdf

Round 3

Reviewer 1 Report

Comments and Suggestions for Authors

Plesae provide a detailed justification and replies to all the points mentioned in our first review (in order).

Comments on the Quality of English Language

OK

Author Response

Thank you, here is our reply.

Author Response File: Author Response.doc

Reviewer 4 Report

Comments and Suggestions for Authors

The work entitled “A kinetic model for the preparation of nano TiO₂ by hydrolysis of TiCl4” studies the particle formation mechanism by using Asen Plus software. The author studied some variables such as water/ethanol ratio, temperature, time, and pH to observe particle size distribution. Nevertheless, this work did not generate new scientific knowledge. It is well known that the mentioned parameters influence the nucleation rate and growth of particles. The theory and practice of particle growth mechanism equations have been already proved some time ago. Now, the scientific community is interested in developing advanced materials with outstanding features for practical applications in the fields of energy, biosensors, bioremediation, medicine, etc,.Because Applied Science is a recognized journal with an impact factor of 2.8, the summited manuscript lacks the merit to be published in this Journal.

Author Response

Thank you for your valuable advice, thank you

Round 4

Reviewer 1 Report

Comments and Suggestions for Authors

Good job.

Comments on the Quality of English Language

Improve.