New Manufacturing Process for Granular Texture Management in Polycrystalline BaM Hexaferrites through the Goethite Crystallite Laths Aspect Ratio, and a Specialized Law of Approach to the Magnetic Saturation for Partly Polarized Uniaxial Materials
Round 1
Reviewer 1 Report
Manuscript: magnetochemistry-2070468
Structural characterization and magnetic properties of polycrystalline BaM hexaferrites with different magnetic texturing grades, manufactured by controlled topotactical reaction, by A. Hoez et al.
The manuscript reports a topotactical-reaction route for the preparation of textured BaM hexaferrite ceramics and different characterization methods for the texturing determination. The ceramics was prepared from two types of reagents, isometric hematite particles and anisotropic goethite particles. Later efficiently enhanced texturing of the BaM ceramics. The texturing was characterized by XRD and from the magnetization measurements using the LAS approach. Authors discuss the conditions enabling using each of two approaches. I suggest to publish the manuscript after authors address some minor comments, listed below:
Line 25–26: names of chemical compounds are written with small letters, i.e., barium hexaferrite and not Barium hexaferrites, strontium hexaferrite and not Strontium hexaferrite.
Line 36: A space is missing "inbetween".
Line 44–45: It is not clear what you meant by a well-textured material always has some misorientation.
Lin 87–88: Typo: Error!Reference Source not found.
Line 381: Figure number is missing.
Author Response
Line 25–26: names of chemical compounds are written with small letters, i.e., barium hexaferrite and not Barium hexaferrites, strontium hexaferrite and not Strontium hexaferrite.
Answer : This was corrected
Line 36: A space is missing "inbetween".
Answer : This was corrected
Line 44–45: It is not clear what you meant by a well-textured material always has some misorientation.
Answer : Thank you, we change this sentence into : It should be made clear, however, that even if the polycrystalline material has a high quality of magnetic texture, there is always some misorientation of the easy axes of magnetization, that could be hardly limited only by applying a strong magnetic field during the compaction process
Lin 87–88: Typo: Error!Reference Source not found.
Answer : This was corrected
Line 381: Figure number is missing.
Answer : This was corrected
Reviewer 2 Report
From reviewing your work, I found it interesting and the results are technically sound, however some points should be improved, and others clarified so that the work can be accepted in this famous and prestigious journal.
1- Authors should carefully review: some sentences show in (Error! Reference source not found.) as in line 87-88 and also some multi spaces are find in the manuscript as in ( line 103, 109, 351….etc.) and some spaces are missed as in (line 242) . The manuscript need fix and double check from the beginning to the end.
2- A good quality image of figure 1 with scale bar visible for the left image should provide.
3- Some figures in low resolution which must be changed as figure 10, figure13.
4- In lines118-119 , the authors stated that “Randomly oriented crystallites of sample BaM-0 (prepared with goethite only) are shown on Fig. 2.a and Fig.2.b shows the stacking of crystallites of sample BaM-100”, however in figure 2 –SEM images-there is no mention to which image is (a) and which one is (b).
5- The authors used Rietveld analysis for confirmation the phase identity but did not stated or listed any fitted parameters as the weighted pattern (Rwp), expected values (Rexp), or the fit goodness index (χ2) which should be stated and some relevant articles are suggested to authors
i) https://iopscience.iop.org/article/10.1088/1402-4896/ac30a7
ii) J. Appl. Cryst. (1969). 2, 65/ 10.1107/s0021889869006558
iii) Crystals 2021, 11, 1153. https://doi.org/10.3390/cryst11101153
6- The word “spectifically” in line 143 is not correct.
7- The author did NOT provide any crystallographic data about the BaM such as lattice parameters, space group,….etc, which could be extracted from the Rietveld refinement also.
8- Line 310 and 311 “we propose to introduce in the relation (xx) an additional factor…..”. There is no relation with name or number (xx) in the manuscript.
9- The corresponding reference must be provided “….in the Stoner and Wolfarth model.” in line 277.
10- There is No number for the referred figure in line 381 (as decribed by MR///MS in Figure ) or the author may rephrase the sentence. The same comment for the sentence in line 400 (…..can be obtained (Figure ))
11- There is mention to figure 12 in the manuscript.
Author Response
First of all we would like to thank you a lot for your careful reviews of our work.
We did our best to modify our manuscript according to your inputs, by which it is upgraded (we expect so) with respect to the first version. Your comments have allowed us to highlight the innovative aspects of our study with respect to the recent literature.
However, because the manuscript has been extensively modified and augmented in many different places, and its structure has been profoundly altered, we have not compiled an exhaustive list of its changes.
The abstract and introduction have been significantly expanded. In particular, we have placed our study in relation to very recent results on the same subject.
Our main inputs focus on the novelty of our study; we show that it is primarily the aspect ratio of the hematite crystals that influences the stacking quality of the BaM particles. It is the value of this parameter, once optimised, that allows to reach a high remanent magnetisation value (Mr/Ms=0.81). This value is significantly higher than the most recent publications in this particular field of self-polarized BaM synthesis using hematite or goethite, and we believe that this value can be further increased by optimizing the heat treatment of the powders after compaction. As the manuscript has been restructured according to the reviewers'comments, this part, which has been greatly expanded compared to the initial version, is now in part 3.1.
What forms parts 3.6 to 3.10 in this new version has not been substantially changed from the same content that was presented in the original version.
The conclusion has been expanded to highlight the novelty of this study.
Please find here below our answers to your comments.
1- Authors should carefully review: some sentences show in (Error! Reference source not found.) as in line 87-88 and also some multi spaces are find in the manuscript as in ( line 103, 109, 351….etc.) and some spaces are missed as in (line 242) . The manuscript need fix and double check from the beginning to the end.
Answer : Thank you. Typo errors were corrected throughout the manuscript.
2- A good quality image of figure 1 with scale bar visible for the left image should provide.
Answer : The quality of this image was improved
3- Some figures in low resolution which must be changed as figure 10, figure13.
Answer : This was corrected
4- In lines118-119 , the authors stated that “Randomly oriented crystallites of sample BaM-0 (prepared with goethite only) are shown on Fig. 2.a and Fig.2.b shows the stacking of crystallites of sample BaM-100”, however in figure 2 –SEM images-there is no mention to which image is (a) and which one is (b).
Answer : This was corrected
5- The authors used Rietveld analysis for confirmation the phase identity but did not stated or listed any fitted parameters as the weighted pattern (Rwp), expected values (Rexp), or the fit goodness index (χ2) which should be stated and some relevant articles are suggested to authors
- i) https://iopscience.iop.org/article/10.1088/1402-4896/ac30a7
- ii) Appl. Cryst. (1969). 2, 65/ 10.1107/s0021889869006558
iii) Crystals 2021, 11, 1153. https://doi.org/10.3390/cryst11101153
Answer : Thank you, these parameters are now listed in the manuscript (new Table 1).
6- The word “spectifically” in line 143 is not correct.
Answer : This was corrected
7- The author did NOT provide any crystallographic data about the BaM such as lattice parameters, space group,….etc, which could be extracted from the Rietveld refinement also.
Answer : Thank you, these parameters are now listed in the manuscript (new Table 1).
8- Line 310 and 311 “we propose to introduce in the relation (xx) an additional factor…..”. There is no relation with name or number (xx) in the manuscript.
Answer : This was corrected
9- The corresponding reference must be provided “….in the Stoner and Wolfarth model.” in line 277.
Answer : This was corrected
10- There is No number for the referred figure in line 381 (as decribed by MR///MS in Figure ) or the author may rephrase the sentence. The same comment for the sentence in line 400 (…..can be obtained (Figure ))
Answer : This was corrected
11- There is mention to figure 12 in the manuscript.
Answer : This was corrected
Reviewer 3 Report
The article is very well written and has good results and discussion especially TEM, SEM & XRD.
It is shown that the ratio 13 hematite: goethite drives the extraction of the samples ( in figure 1 TEM and Figure 2 SEM, the authors have not added the EDS/EDX results to show the elemental analysis to establish the proper distribution of extraction ratio).
Author Response
It is shown that the ratio 13 hematite: goethite drives the extraction of the samples ( in figure 1 TEM and Figure 2 SEM, the authors have not added the EDS/EDX results to show the elemental analysis to establish the proper distribution of extraction ratio).
Answer : Thank you for your comment. EDS/EDX results are not provided because EDS measurements would not allow to distinguished the BaFe12O19 particles formed from hematite than these formed from goethite. Rietveld analysis allows to ensure that the material is single phase.
Round 2
Reviewer 2 Report
The manuscript can be accepted in present form.
