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The impact of reaction time on the hierarchical structure of mesoporous silica synthesized via modified stöber method

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Abstract

An investigation was conducted to observe the transformation of mesoporous silica nanoparticles (MSN) prepared using the modified Stober method with a cetyltrimethylammonium bromide (CTAB) template and varying aging periods. The hierarchical structure of the mesoporous silica nanostructure was analyzed using electron microscopy (FE-SEM and TEM) measurements, N2 adsorption, and small-angle X-rays scattering (SAXS). A comprehensive study using these instruments revealed that aging time significantly affected the morphology, pore structures, surface area, and pore size of the particles. It was observed that mesoporous silica grown in diverse morphologies from spherical nanoparticles, irregular particles, and nano-rods with an increase in aging time for 12 h, 18 and 24 h respectively. The SAXS and N2 adsorption measurements unveiled an intriguing relationship where the pore radius and surface area of MSN decreased with longer maturation times, reducing from 4.77 nm to 2.65 nm and from 849.43 m²/g to 572.85 m²/g, respectively. The results of the SAXS analysis also indicated a change in the pore structure due to prolonged reaction time, transitioning from a hexagonal structure to a loss of its orderedness. These findings play a crucial role in enhancing our understanding of how aging time influences the formation mechanism of MSNs for their diverse applications.

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Acknowledgements

The authors are thankful to the funding from research program of the product of nuclear technological innovation 2023 (D3324), from Research Organization of Nuclear Power- National Research and Innovation Agency-Indonesia.

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Authors and Affiliations

  1. Research Center for Nuclear Beam Analytics Technology, Research Organization for Nuclear Energy, National Research and Innovation Agency, Serpong, Tangerang Selatan, 15314, Indonesia

    Muflikhah & Arum Patriati

  2. Directorate of Nuclear Facility Management, National Research and Innovation Agency, Serpong, 15314, Tangerang Selatan, Indonesia

    Nadi Suparno & Wildan Zakiah Lbs

  3. Polytechnic Institute of Nucelar Technology, National Research and Innovation Agency, Yogyakarta, Indonesia

    Maria Christina Prihatiningsih

  4. Synchrotron Light Research Institute (SLRI), 111 University Avenue, Muang District, Nakhon Ratchasima, 30000, Thailand

    Siriwat Soontaranoon

  5. Research Center for Advanced Materials, National Research and Innovation Agency, Serpong, 15314, Tangerang Selatan, Indonesia

    Ade Mulyawan

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  1. Muflikhah
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Contributions

M: Conceptualization, performed the experiments and analysis, wrote the main original draft. N.S: Data curation. W.Z.L: Performed the experiments. S.S: Data curation of SAXS. M.C.P: Supervision, writing - review. A.M: Writing - review, prepared figures. A.P: Data curation and analysis, writing - original draft and review.

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Correspondence to Muflikhah.

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Muflikhah, Suparno, N., Lbs, W.Z. et al. The impact of reaction time on the hierarchical structure of mesoporous silica synthesized via modified stöber method. J Porous Mater 31, 969–977 (2024). https://doi.org/10.1007/s10934-024-01574-z

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