Development of bacterial cellulose–ZnO–MWCNT hybrid membranes: a study of structural and mechanical properties

Self-supported and flexible bacterial cellulose (BC) based hybrid membranes were synthesized and decorated with zinc oxide/multi-walled carbon nanotube (ZnO–MWCNT) composite additives in order to modify and tune their surface and bulk properties. Two types of ZnO–MWCNT additives with different morphologies were used in a wide concentration range from 0 to 90% for BC-based hybrids produced by filtration. The interaction between BC and ZnO–MWCNT and the effect of concentration and morphology of additives on the properties like zeta potential, hydrophilicity, electrical conductivity, etc. would be an important factor in various applications. Furthermore, the as-prepared hybrid membranes were characterized with the use of scanning electron microscopy (SEM), focused ion beam scanning electron microscopy (FIB-SEM), energy dispersive X-ray spectroscopy (EDS), X-ray powder diffraction (XRD) and surface area measurement (BET). Applying the presented synthesis routes, the surface properties of BC-based membranes can be tailored easily. Results reveal that the as-prepared BC–ZnO–MWCNT hybrid membranes can be ideal candidates for different kinds of applications, such as water filtration or catalysts.

3. Raman spectra shows the peaks of MWCNT. THey are assigned to D-, G-and G*-bands. Please explain the physical meaning of these bands and provide a reference to support. Figures 1d and 1f are not corresponding to the figures 1c and 1f, or 1d and 1e. It is obvious that the shape of the ZNO particle in Figure 1g is very different as that in Figure 1f. Please provide a map that can match SEM micrograph. 5. It is recommended SEM FIB preparing to obtain an XTEM specimen followed by higher magnification TEM investigation in order to provide better proof of MWCNT in terms of lattice fringes showing the layer number of the walls, the inner and outer diameter of the CNT.

SEM-Element map in
it is recommended to accept it on the condition that the above revision request was carefully responded by the authors.

Decision letter (RSOS-200592.R0)
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Dear Dr Nemeth: Title: Development of bacterial cellulose-MWCNT/ZnO hybrid membranes: a study of structural and mechanical properties Manuscript ID: RSOS-200592 Thank you for submitting the above manuscript to Royal Society Open Science. On behalf of the Editors and the Royal Society of Chemistry, I am pleased to inform you that your manuscript will be accepted for publication in Royal Society Open Science subject to minor revision in accordance with the referee suggestions. Please find the reviewers' comments at the end of this email.
The reviewers and handling editors have recommended publication, but also suggest some minor revisions to your manuscript. Therefore, I invite you to respond to the comments and revise your manuscript.
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Supplementary files will be published alongside the paper on the journal website and posted on the online figshare repository (https://figshare.com). The heading and legend provided for each supplementary file during the submission process will be used to create the figshare page, so please ensure these are accurate and informative so that your files can be found in searches. Files on figshare will be made available approximately one week before the accompanying article so that the supplementary material can be attributed a unique DOI. ********************************************** RSC Associate Editor: Comments to the Author: have authors studied the doping concentration dependence studies. ********************************************** Reviewer comments to Author: Reviewer: 1 Comments to the Author(s) The manuscript by Nemeth et.al. provides that the structural and mechanical properties of BC-MWCNT/ ZnO are tailored by impregnation and solvothermal methods. These two methods are key procedures for tune and decorate the BC-MWCNT/ZnO hybrid membranes. Thus, Author should give the detail procedure of impregnation and solvothermal methods in Materials and Methods section of the manuscript. Even though it cited in the references 22. The written conclusions is not specific and clear to understand, that which method is provided the finely tuned or excellent morphology of hybrid membranes. Need to rewrite the conclusions before it is considered for the publications. Also it is difficult to understand and follow the given abbreviations of developed materials, need to change such as BC-ZnO-MWCNT/Imp …… instead of… BC-MWCNT/ZnO-IMP (page no 5, line 14) BC-ZnO-MWCNT/Solv …… instead of… BC-MWCNT/ZnO-SOLVO (page no 5, line 14) Because both are derived from different methods and not the part of hybrid membranes. Overall the work is very important contributions in the field surface modifications of the membrane. Research article can be consider for the publication after revision of above mentioned comments.

Reviewer: 2
Comments to the Author(s) Minor revision is suggested as below: 1. The amorphous status of ZnO in the composite was verified by X-ray diffraction. It is recommended to obtain selected area electron diffraction of the amorphous ZnO. X-ray diffraction is a mean result of both ZnO NPs and the surrounding materials. TEM can give you an electron diffraction of a much small area.
2. When identifying ZNO crystal structure, the diffracted angles are provided and look like matching well with published data. But it would be very help for the lattice parameters of ZnO crystal can be provided in the manuscript for the convenience of readers' understanding.
3. Raman spectra shows the peaks of MWCNT. THey are assigned to D-, G-and G*-bands. Please explain the physical meaning of these bands and provide a reference to support. Figures 1d and 1f are not corresponding to the figures 1c and 1f, or 1d and 1e. It is obvious that the shape of the ZNO particle in Figure 1g is very different as that in Figure 1f. Please provide a map that can match SEM micrograph. 5. It is recommended SEM FIB preparing to obtain an XTEM specimen followed by higher magnification TEM investigation in order to provide better proof of MWCNT in terms of lattice fringes showing the layer number of the walls, the inner and outer diameter of the CNT.

SEM-Element map in
it is recommended to accept it on the condition that the above revision request was carefully responded by the authors.

Author's Response to Decision Letter for (RSOS-200592.R0)
See Appendix A.

Decision letter (RSOS-200592.R1)
We hope you are keeping well at this difficult and unusual time. We continue to value your support of the journal in these challenging circumstances. If Royal Society Open Science can assist you at all, please don't hesitate to let us know at the email address below.
Dear Dr Nemeth: Title: Development of bacterial cellulose-ZnO-MWCNT hybrid membranes: a study of structural and mechanical properties Manuscript ID: RSOS-200592.R1 It is a pleasure to accept your manuscript in its current form for publication in Royal Society Open Science. The chemistry content of Royal Society Open Science is published in collaboration with the Royal Society of Chemistry.
The comments of the reviewer(s) who reviewed your manuscript are included at the end of this email.
Thank you for your fine contribution. On behalf of the Editors of Royal Society Open Science and the Royal Society of Chemistry, I look forward to your continued contributions to the Journal.