4.7 Article

Unveiling unique structural features of the YNU-5 aluminosilicate family

Journal

MICROPOROUS AND MESOPOROUS MATERIALS
Volume 317, Issue -, Pages -

Publisher

ELSEVIER
DOI: 10.1016/j.micromeso.2021.110980

Keywords

Zeolites; Electron diffraction tomography (EDT); Structure analysis; Rietveld refinement; Spherical aberration-corrected STEM

Funding

  1. SPST of ShanghaiTech University [EM02161943]
  2. National Natural Science Foundation of China [NFSC21850410448, NSFC21835002]
  3. Spanish Ministry of Science under the Ramon y Cajal Program [RYC2018-024561-I]
  4. regional government of Aragon [DGA E13_20R]
  5. Japan Science and Technology Agency (JST) [JPMJSC18C4]
  6. Japan Society for the Promotion of Science (JSPS) [19H02513]

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This study investigated the structures of YNU-5 zeolites using various techniques, with a focus on advanced electron microscopy methods. The space group for the YNU-5 zeolites was determined to be Cmmm, showing higher symmetry than previously reported. Additionally, Rietveld refinement of synchrotron Powder X-ray diffraction data provided precise information on the framework and the location of organic species, cations, and water.
YNU-5 (YFI type) is the first zeolite reported with interconnected 12-, 12-, and 8-ring pores showing a remarkable catalytic potential towards the dimethyl ether (DME)-to-olefin reaction. In this work, the structures of the as-synthesized, calcined and dealuminated YNU-5 zeolites, were investigated by various techniques with special emphasis on advanced electron microscopy methods. The frameworks of the three materials were solely determined by three-dimension electron diffraction tomography, and the space group for the three of them was determined to be Cmmm, which is of higher symmetry than the previous reported result. Rietveld refinement was performed against synchrotron Powder X-ray diffraction data in order to obtain precise information of the framework and to locate the organic species, cations and water. Additionally, spherical aberration-corrected scanning transmission electron microscopy was employed to study the local fine structure and to indicate surface reconstruction associated to the displacement of the vacancies through the dealumination process. Finally, a minor phase, whose structure was solved by electron microscopy was found to be MSE framework type, appeared in all the three YNU-5 materials. Overall, the electron microscopy analyses reported in the present work provide additional information regarding the YNU-5 structure in terms of space group determination, additional surface terminations and the identification of a minor phase.

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