Research ArticleMATERIALS SCIENCE

Liquid dispersions of zeolite monolayers with high catalytic activity prepared by soft-chemical exfoliation

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Science Advances  20 Mar 2020:
Vol. 6, no. 12, eaay8163
DOI: 10.1126/sciadv.aay8163
  • Fig. 1 In situ XRD of concentrated layers in water (black line) and the square of structure factor F (red line) calculated based on the MWW structure.

    The observed deviation between the calculated and experimental intensities at higher 2θ angles is due to amorphous halo from water because the glue-like sample recovered via centrifugation contains large amount of the solvent. Damping the wavy profile at a higher angular range may be involved by some structural disorder.

  • Fig. 2 AFM topography image of diluted colloidal MCM-56.

    Zeolite suspension deposited on a silicon support modified with polyethylenimine (PEI) solution (A) and height profile along the marked line (B).

  • Fig. 3 Crystalline structure of MCM-56 monolayers separated from the colloidal suspensions.

    (A and B) TEM image and SAED pattern along the c-axis, showing the whole nanosheet to be a single crystal. (C and D) HRTEM images, atomic models, and simulated TEM images of in-plane (C) and edge-view (D) structures.

  • Fig. 4 Zeolite film with a diameter of 18 mm obtained from the colloidal dispersion.

    (A) photograph and (B) XRD data, which show only the basal reflections and no peaks associated with the in-plane periodicity, confirming that zeolite nanosheets are stacked with their faces parallel to the film surface. Photo credit: Yeji Song, NIMS.

Supplementary Materials

  • Supplementary material for this article is available at http://advances.sciencemag.org/cgi/content/full/6/12/eaay8163/DC1

    Fig. S1. SAXS profiles for MCM-56 samples in TBAOH solutions at different concentrations (10, 8, 6, and 4 weight %).

    Fig. S2. Graphical illustration of the in situ XRD setup and measurement.

    Fig. S3. The atomic positions used in structure factor calculation for the MWW layer.

    Fig. S4. In-plane XRD data for monolayers from the MCM-56 colloid deposited onto a Si substrate.

    Fig. S5. Photographs and cross-sectional SEM images of the MWW zeolite film produced from the colloidal suspension of MCM-56 layers.

    Fig. S6. Selected powder XRD, TEM, and nitrogen adsorption/desorption characteristics of the materials obtained from the MCM-56 colloid suspensions.

    Fig. S7. Catalytic activity of the original MCM-56 and the zeolite recovered from colloid by flocculation with 1 M ammonium nitrate: Conversion of benzyl alcohol in alkylation of mesitylene.

    Table S1. Representative acidic and textural properties of the starting MCM-56 zeolites and the products obtained from the colloidal dispersions by flocculation with 1 M ammonium nitrate solution and the Al-oxo-13 cluster ions.

  • Supplementary Materials

    This PDF file includes:

    • Fig. S1. SAXS profiles for MCM-56 samples in TBAOH solutions at different concentrations (10, 8, 6, and 4 weight %).
    • Fig. S2. Graphical illustration of the in situ XRD setup and measurement.
    • Fig. S3. The atomic positions used in structure factor calculation for the MWW layer.
    • Fig. S4. In-plane XRD data for monolayers from the MCM-56 colloid deposited onto a Si substrate.
    • Fig. S5. Photographs and cross-sectional SEM images of the MWW zeolite film produced from the colloidal suspension of MCM-56 layers.
    • Fig. S6. Selected powder XRD, TEM, and nitrogen adsorption/desorption characteristics of the materials obtained from the MCM-56 colloid suspensions.
    • Fig. S7. Catalytic activity of the original MCM-56 and the zeolite recovered from colloid by flocculation with 1 M ammonium nitrate: Conversion of benzyl alcohol in alkylation of mesitylene.
    • Table S1. Representative acidic and textural properties of the starting MCM-56 zeolites and the products obtained from the colloidal dispersions by flocculation with 1 M ammonium nitrate solution and the Al-oxo-13 cluster ions.

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