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Facile synthesis to tune size, textural properties and fiber density of dendritic fibrous nanosilica for applications in catalysis and CO2 capture

Nature Protocols volume 14, pages 2177–2204 (2019)Cite this article

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Abstract

Morphology-controlled nanomaterials such as silica play a critical role in the development of technologies for use in the fields of energy, environment (water and air pollution) and health. Since the discovery of Stöber’s silica, followed by the discovery of mesoporous silica materials (MSNs) such as MCM-41 and SBA-15, a surge in the design and synthesis of nanosilica with various sizes, shapes, morphologies and textural properties (surface area, pore size and pore volume) has occurred. Dendritic fibrous nanosilica (DFNS; also known as KCC-1) is one of the recent discoveries in morphology-controlled nanomaterials. DFNS shows exceptional performance in large numbers of fields, including catalysis, gas capture, solar energy harvest, energy storage, sensors and biomedical applications. This material possesses a unique fibrous morphology, unlike the tubular porous structure of various conventional silica materials. It has a high surface area to volume ratio, with improved accessibility to the internal surface, tunable pore size and pore volume, controllable particle size and, importantly, improved stability. However, synthesis of DFNS with controllable size, textural properties and fiber density is still tricky because of several of the steps involved. This protocol provides a comprehensive step-wise description of DFNS synthesis and advice regarding how to control size, surface area, pore size, pore volume and fiber density. We also provide details of how to apply DFNS in catalysis and CO2 capture. Detailed characterization protocols for these materials using scanning electron microscopy (SEM), transmission electron microscopy (TEM), nitrogen adsorption and thermal gravimetric analysis (TGA) studies are also provided.

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Fig. 1: Schematic illustration of DFNS synthesis.
Fig. 2
Fig. 3: SEM images and particle-size distribution.
Fig. 4: TEM images of synthesized DFNSs under different conditions at large scale.
Fig. 5: Characteristics of DFNSs.
Fig. 6: SEM images and particle-size distribution.
Fig. 7: TEM images of synthesized DFNSs using different co-surfactants at small scale.
Fig. 8: Characteristics of DFNSs.
Fig. 9
Fig. 10: Typical results seen for DFNS-TEPAads.
Fig. 11: Typical results seen for DFNS-NH2 and DFNS-NH2/Pd.
Fig. 12
Fig. 13: Typical results seen for DFNS-TEPAads.

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All data generated or analyzed during this study are included in this published article.

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Acknowledgements

This work was supported by the Department of Atomic Energy (DAE), Government of India. We would like to also thank Indo-France CEFIPRA and SHELL Industries for funding that partially supported this work. We acknowledge the EM, XRD and NMR Facility of TIFR, Mumbai.

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Authors and Affiliations

  1. Department of Chemical Sciences, Tata Institute of Fundamental Research (TIFR), Mumbai, India

    Ayan Maity, Rajesh Belgamwar & Vivek Polshettiwar

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  1. Ayan Maity
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Contributions

V.P. proposed the research direction and guided the project. A.M. and V.P. developed the protocol. A.M. and R.B. performed the experiments. A.M. and V.P. drafted the manuscript. All authors contributed to the manuscript. We thank S. Rawool and M. Dhiman for their support during the preparation of this protocol.

Corresponding author

Correspondence to Vivek Polshettiwar.

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The authors declare no competing interests.

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Journal peer review information: Nature Protocols thanks Ling Chao and other anonymous reviewer(s) for their contribution to the peer review of this work.

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Related links

Key references using this protocol

Maity, A. & Polshettiwar, V. ChemSusChem 10, 3866−3913 (2017): https://onlinelibrary.wiley.com/doi/full/10.1002/cssc.201701076

Polshettiwar, V., Cha, D., Zhang, X. & Basset, J. M. Angew. Chem. Int. Ed. 49, 9652−9656 (2010): https://onlinelibrary.wiley.com/doi/full/10.1002/anie.201003451

Key data used in this protocol

Maity, A. & Polshettiwar, V. ACS Appl. Nano Mater. 1, 3636–3643 (2018): https://pubs.acs.org/doi/10.1021/acsanm.8b00761

Maity, A., Das, A., Sen, D., Mazumder, S. & Polshettiwar, V. Langmuir 33, 13774−13782 (2017): https://pubs.acs.org/doi/10.1021/acs.langmuir.7b02996

Singh, B. & Polshettiwar, V. J. Mater. Chem. A 4, 7005–7019 (2016): https://pubs.rsc.org/is/content/articlehtml/2016/ta/c6ta01348a

Fihri, A., Cha, D., Bouhrara, M., Almana, N. & Polshettiwar, V. ChemSusChem 5, 85–89 (2012): https://onlinelibrary.wiley.com/doi/full/10.1002/cssc.201100379

Maity, A. & Polshettiwar, V. ChemSusChem 10, 3866−3913 (2017): https://onlinelibrary.wiley.com/doi/full/10.1002/cssc.201701076

Polshettiwar, V., Cha, D., Zhang, X. & Basset J. M. Angew. Chem. Int. Ed. 49, 9652−9656 (2010): https://onlinelibrary.wiley.com/doi/full/10.1002/anie.201003451

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Maity, A., Belgamwar, R. & Polshettiwar, V. Facile synthesis to tune size, textural properties and fiber density of dendritic fibrous nanosilica for applications in catalysis and CO2 capture. Nat Protoc 14, 2177–2204 (2019). https://doi.org/10.1038/s41596-019-0177-z

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