PAN—Composite Electrospun-Fibers Decorated with Magnetite Nanoparticles
, Bayan Kaidar 1,2, Aigerim Imash 1,2,* and Aidos Lesbayev 1,3Round 1
Reviewer 1 Report
This reports the preparation of Fe3O4 doped PAN fibers, the research is interesting. However, revisions are needed to improve the quality of manuscript.
1. The loading of Fe3O4 should be optimized, along with their PXRD, SEM.
2. SEM images of PAM/Fe3O4 recorded under different magnification should be provided
3. TEM studies of PAM/Fe3O4 are required.
4. A potential application should be proposed and demonstrated, to show the future of reported method.
5. Some references are encouraged to cite, such as (1) Rare Metals. 2020, 39(11):1333―1340.https://doi.org/10.1007/s12598-017-0940-7. (2) Chinese Chemical Letters, 2022, 33, 141-152. https://doi.org/10.1016/j.cclet.2021.08.097. (3) Chemical Engineering Journal, 2022, 431, 134343. https://doi.org/10.1016/j.cej.2021.134343
Author Response
1. The loading of Fe3O4 should be optimized, along with their PXRD, SEM.
We agree with the remark. Unfortunately, PXRD is not available in our lab. There is no option to include these results. SEM images of magnetite nanoparticles were included (Fig. 2a).
2. SEM images of PAM/Fe3O4 recorded under different magnification should be provided.
We agree with the remark. SEM images of PAN/magnetite fibers at various magnifications were included (Fig. 5a, b).
3. TEM studies of PAN/Fe3O4 are required.
Unfortunately, the diameter of the PAN/magnetite fibers is too large to be scanned by TEM and these studies have not been carried out.
4. A potential application should be proposed and demonstrated, to show the future of reported method.
Agree with the remark. This information has been included. Links [1-7, 36-43]
5. Some references are encouraged to cite, such as
(1) Rare Metals. 2020, 39(11):1333-1340. https://doi.org/10.1007/s12598-017-0940-7.
(2) Chinese Chemical Letters, 2022, 33, 141-152. https://doi.org/10.1016/j.cclet.2021.08.097.
(3) Chemical Engineering Journal, 2022, 431, 134343. https://doi.org/10.1016/j.cej.2021.134343
We agree with the remark. This information has been included.
Reviewer 2 Report
Dear author
It gets me pleasure to reviewing paper.entitled PAN - composite electrospun-fibers decorated with magnetite nanoparticles at Magnetochemistry journal.
The manuscript illustrates preparation of magnetic iron nanoparticles via chemical condensation and incorporation these magnetic nanoparticles with polyacrylonitrile PAN. Different spectrophotometric analysis used to measure interaction and morphology of synthesized nanoparticles and electrospun fiber loaded magnetic particles as SEM. TEM. PS and XRD.
The manuscript need major revision and more analysis
Firstly lack of experiments as FTIR
Lack of measurement as Magnetism
Lack of systematic study in the manuscript
There is no novelty
For introduction part
Long introduction part to hole manuscript
For methods
It lacks of important analysis for electrospinning as measuring conductivity viscosity, and lack of systematic study as changing polymer ratios, conductivity, distance and effect of these factors on electrospinning process
There is no application in the manuscript
For conclusion
Actually it needed to extend, it's to short to the hole manuscript as result of lack analysis
Lack of Novelty many reports speaks about preparation of PAN nanofiber loaded iron magnetic particles, so what is new
We recommend major revision with more analysis.
Author Response
The manuscript need major revision and more analysis
Dear reviewer. The authors thank you for the revision of the article, which has significantly improved its quality.
Firstly lack of experiments as FTIR
Unfortunately, our laboratory does not have an FTIR device to carry out research. However, the authors included the results of EDS analysis and hope that XRD and EDS analyzes will be sufficient to identify samples. An EDS analysis for magnetite was included (Fig. 3a).
Lack of measurement as Magnetism
We agree with the remark. Data on the determination of the magnetic properties of magnetite nanoparticles were included. Unfortunately, there are no data on the magnetic properties of PAN/magnetite fibers due to the fact that the studies were carried out in a foreign laboratory and now there is no possibility of conducting an analysis due to the unstable political situation. The results of measuring the magnetism of the Fe3O4 nanoparticles were included (Fig. 4).
Lack of systematic study in the manuscript
We agree with the remark. The structure of the article was considered and additional research results were introduced. According to the comments of the reviewers, corrections and additions were made. The authors hope that this has improved the article.
There is no novelty
The authors hope that the main novelty and value of the work lies in the development of a simple technique for obtaining PAN/magnetite composite fibers using a simple and cheap chemical deposition method. And the proposed conditions of the electrospinning process make it possible to obtain stable fibers without the inclusion of defects.
For introduction part
Long introduction part to hole manuscript
We agree with the remark, but the authors wanted to consider the most scientifically interesting and most recent works (2019-2021) in the field of magnetic nanomaterials. And we would like to leave an introduction so that readers understand the importance and relevance of the development of magnetic nanomaterials.
For methods
It lacks important electrospinning analysis such as conductivity, viscosity measurements, as well as the lack of systematic studies on the change in polymer ratio, conductivity, distance and the influence of these factors on the electrospinning process.
We agree with the remark. Studies on the influence of the concentration of the polymer solution, as well as on the influence of the conditions of the electrospinning process (distance, voltage, etc.) have been carried out. The effect of concentration from 7 wt. % up to 13 wt. %. It was found that the optimal concentration is 7 wt. %, at lower and higher concentrations, spherical and elongated structures are formed in the fibers, which indicates the instability of the electrospinning process. All these studies were summarized in the project report, but since they have no scientific value these results were not included. A detailed explanation of defect formation can be found in [Seeram Ramakrishna, Kazutoshi Fujihara, Wee-Eong Teo.Teik-Cheng Lim & Zuwei Ma. AN INTRODUCTION TO ELECTROSPINNING AND NANOFIBERS. World Scientific Publishing Co. Pte. Ltd. 2005. ISBN 981-256-415-2. 382p].
There is no application in the manuscript
The obtained fibers are used for the manufacture of composite materials by vacuum infusion from PAN/magnetite fibers and epoxy resin. However, these studies are not yet completed.
For conclusion
It lacks of important analysis for electrospinning as measuring conductivity viscosity, and lack of systematic study as changing polymer ratios, conductivity, distance and effect of these factors on electrospinning process
Actually it needed to extend, it's to short to the hole manuscript as result of lack analysis
We agree with the remark. The conclusion has been extended.
Lack of Novelty many reports speaks about preparation of PAN nanofiber loaded iron magnetic particles, so what is new
We do not in any way say that our results are superior to those of other scientists and we fully respect all research. The main difference of this work from similar articles is a more uniform distribution of magnetite nanoparticles over the fiber structure. We reviewed a number of works including [DOI: 10.3390/s21237873, https://doi.org/10.3390/polym14030533, and other articles] and came to the conclusion that the results obtained by us could be useful to researchers in obtaining PAN fibers/ magnetite by electrospinning. Because at the specified process parameters, stable fibers are formed without defects in the form of spherical inclusions or fiber breaks. And the use of a simple and cheap method of chemical condensation to obtain magnetite nanoparticles makes the proposed method more economically viable.
We recommend major revision with more analysis.
The authors once again thank you for the careful review of the presented article.
Author Response File: 
Author Response.pdf
Reviewer 3 Report
The current work focuses on PAN-composite electrospun-fibers decorated with magnetite nanoparticles. The author’s some effort into the manuscript, but major issues should be addressed. Extensive editing of English language and style required.
Abstract
- The first appearance of abbreviations should have a full definition e.g. PAN
Introduction
- The introduction doesn’t provide sufficient background, and all relevant references are not included.
https://doi.org/10.3390/polym14030533
https://doi.org/10.1002/pc.24647
https://doi.org/10.1515/ntrev-2022-0116
- Line 24-30, all those applications of magnetic materials need more citations
- Line 39-42, a very long sentence; please rephrase it to be shorter
“The review [2] represents the methods of synthesis of magnetic nanoparticles, 90% of which are chemical methods; the issues of nanoparticles modification by organic and inorganic compounds, polymers and bioactive molecules are discussed; methods of protein immobilization using magnetic nanoparticles, mainly based on Fe3O4”
- Line 45-48, a very long sentence; please rephrase it to be shorter
“In paper [4] the synthesis of Fe3O4/SiO2 and CoFe2O4 /SiO2 structures by co-precipitation or hydrothermal synthesis of Fe3O4 with further coating their surface with a layer of silicon dioxide and functionalization with 3-aminopropyl- triethoxysilane was shown.”
- Line 118, correct typo FeCl3•6H2O and FeCl2•4H2O
-The novelty of this work is not highlighted and it was not clear the author's contribution in comparison to other previous works.
Materials and methods section
- The impurities of the used materials should be inserted
- Line 143-144, please correct this sentence
“Method of obtaining Fe3O4 magnetite nanoparticles and composite fibers Synthesis of Fe3O4 magnetite nanoparticles”
- What is the condition for XRD analysis, and scanning rate? Range?
Results and discussion
The main problem in the manuscript is that the authors show only results without more interpretations of it or confirmation by citation. More details are required to explain the obtained results.
- Line 187-188, “Particles of 50 nm and larger are also seen in the image, but the authors believe that these dimensions are due to overlapping of the particles.” some interpretation could be added to support it
e.g. “The agglomeration of magnetic particles is due to the presence of high surface energy between the prepared magnetic nanoparticles and the presence of magnetic dipole-dipole interactions“ https://doi.org/10.1080/01932691.2019.1635025
- Line 183-184, “The predominant fraction of particles has sizes from 6 to 16 nm” but in the abstract “It was shown that homogeneous Fe3O4 magnetite nanoparticles with particle sizes of 8-25 nm could be synthesized by this method.” So which one is the right?
- Line 208-211, “Comparison of PAN and PAN/Fe3O4 fibers shows that the presence of magnetite in the solution composition leads to a decrease in the diameter of the fibers formed as a result of electrospinning: for PAN fibers dav = 0.924 μm, for PAN/Fe3O4 fibers dav = 0.345 μm.”
Is there any interpretation or details on this observation why decreasing diameter in the presence of magnetite nanoparticles? This claim should have more details and interpretation.
- VSM analysis is required to investigate the magnetic properties of the fabricated fiber
- TGA analysis is required to investigate the effect of magnetite nanoparticles on the thermal stability of the fabricated fiber
Author Response
Dear reviewer. The authors would like to thank you for the revision of the article, which has significantly improved its quality.
Abstract
- The first appearance of abbreviations should have a full definition e.g. PAN
We agree with the remark. The full definition of the abbreviation has been included.
Introduction
- The introduction doesn’t provide sufficient background, and all relevant references are not included.
https://doi.org/10.3390/polym14030533 [16]
https://doi.org/10.1002/pc.24647 [17]
https://doi.org/10.1515/ntrev-2022-0116 [23]
We agree with the comment. This information has been included.
- Line 24-30, all those applications of magnetic materials need more citations
We agree with the remark. This information has been included. References [1-7]
- Line 39-42, a very long sentence; please rephrase it to be shorter
“The review [2] represents the methods of synthesis of magnetic nanoparticles, 90% of which are chemical methods; the issues of nanoparticles modification by organic and inorganic compounds, polymers and bioactive molecules are discussed; methods of protein immobilization using magnetic nanoparticles, mainly based on Fe3O4”
We agree with the remark. The proposal has been divided into 3 parts: «The review [2] represents the methods of synthesis of magnetic nanoparticles, 90% of which are chemical methods. The issues of nanoparticles modification by organic and inorganic compounds, polymers and bioactive molecules are discussed. Also, methods of protein immobilization using magnetic nanoparticles, mainly based on Fe3O4 are discussed.»
- Line 45-48, a very long sentence; please rephrase it to be shorter
“In paper [4] the synthesis of Fe3O4/SiO2 and CoFe2O4 /SiO2 structures by co-precipitation or hydrothermal synthesis of Fe3O4 with further coating their surface with a layer of silicon dioxide and functionalization with 3-aminopropyl- triethoxysilane was shown.”
We agree with the remark. The sentence has been rephrased.
In paper [4] the synthesis of Fe3O4/SiO2 and CoFe2O4/SiO2 structures by co-precipitation or hydrothermal synthesis of Fe3O4 was shown. Obtained Fe3O4 was coated surface with a layer of silicon dioxide and functionalization with 3-aminopropyl-triethoxysilane was carried out.
- Line 118, correct typo FeCl3•6H2O and FeCl2•4H2O
This ratio was mentioned in the article [https://doi.org/10.17073/1609-3577-2013-4-22-29.]
-The novelty of this work is not highlighted and it was not clear the author's contribution in comparison to other previous works.
The authors hope that the main novelty and value of the work lies in the development of a simple technique for producing PAN/magnetite composite fibers using a simple and cheap chemical deposition method. And the proposed conditions of the electrospinning process make it possible to obtain stable fibers without the inclusion of defects.
Materials and methods section
- The impurities of the used materials should be inserted
Unfortunately, the reagent data sheets do not specify which impurities may be present and in what quantities.
- Line 143-144, please correct this sentence
“Method of obtaining Fe3O4 magnetite nanoparticles and composite fibers Synthesis of Fe3O4 magnetite nanoparticles”
We agree with the remark. Corrected. That was a typo.
- What is the condition for XRD analysis, and scanning rate? Range?
We agree with the remark. A detailed description of the research parameters have been included in the section "Analytical methods of investigation of Fe3O4 magnetite nanoparticles and composite fibers".
Results and discussion
The main problem in the manuscript is that the authors show only results without more interpretations of it or confirmation by citation. More details are required to explain the obtained results.
- Line 187-188, “Particles of 50 nm and larger are also seen in the image, but the authors believe that these dimensions are due to overlapping of the particles.” some interpretation could be added to support it
e.g. “The agglomeration of magnetic particles is due to the presence of high surface energy between the prepared magnetic nanoparticles and the presence of magnetic dipole-dipole interactions“ https://doi.org/10.1080/01932691.2019.1635025
We agree with the remark. The proposed information has been included. And additional information has also been included.
- Line 183-184, “The predominant fraction of particles has sizes from 6 to 16 nm” but in the abstract “It was shown that homogeneous Fe3O4 magnetite nanoparticles with particle sizes of 8-25 nm could be synthesized by this method.” So which one is the right?
We agree with the remark. It was a typo. 6-16 is the correct value.
- Line 208-211, “Comparison of PAN and PAN/Fe3O4 fibers shows that the presence of magnetite in the solution composition leads to a decrease in the diameter of the fibers formed as a result of electrospinning: for PAN fibers dav = 0.924 μm, for PAN/Fe3O4 fibers dav = 0.345 μm.”
Is there any interpretation or details on this observation why decreasing diameter in the presence of magnetite nanoparticles? This claim should have more details and interpretation.
We agree with the remark Additional references have been included.
- VSM analysis is required to investigate the magnetic properties of the fabricated fiber
- TGA analysis is required to investigate the effect of magnetite nanoparticles on the thermal stability of the fabricated fiber
Unfortunately. At present, it is not possible to carry out additional tests due to the lack of a TGA and VSM device and the repair work that is being carried out at the Institute.
Author Response File: Author Response.pdf
Round 2
Reviewer 1 Report
The authors should take a more serious action to revise the manuscript.
Reviewer 3 Report
Accept in present form
