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Microscopy of Nanoporous Crystals

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Abstract

Nanoporous crystals are widely studied and used for applications in \(\mathrm{H_{2}}\) storage, \(\mathrm{CO_{2}}\) capture, petrochemical catalysis and many other applications, yet the imaging of their atomic structure has proven difficult because of their radiation sensitivity and the small size of these microcrystals. This chapter describes the development of the new modes of electron microscopy needed to study them, and compares these with traditional methods such as x-ray diffraction. This class of materials has traditionally been dominated by the zeolites and zeotype materials, but has recently been expanded to include meso-/macroporous crystals and other new framework structures (MOFs, ZIFs COFs, etc.). Using different building blocks or units, versatile crystal structures have been synthesized for various applications. Their properties and functions are governed primarily by periodic arrangements of pores and/or cavities and their surroundings with various atomic moieties inside crystals. In this chapter, electron microscopy studies of nanoporous materials are discussed from different perspectives. Special attention is paid to the observation of fine defect structures, through careful analysis of electron diffraction, high-resolution images and spectroscopy data. The experimental conditions for imaging beam-sensitive materials, such as MOFs, are described. The contents have been divided into sections based on the types of materials and their geometric features. Examples of structure analysis of various nanoporous materials are given and discussed. New technical developments and existing challenges are described.

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References

  • O. Terasaki, T. Ohsuna, Z. Liu, Y. Sakamoto, A.E. Garcia-Bennett: Structural study of meso-porous materials by electron microscopy. In: Proc. Meet. Mesoporous Cryst. Relat. Nano-Struct. Mater (Elsevier, Amsterdam 2004) pp. 261–288

    Google Scholar 

  • C. Xiao, N. Fujita, K. Miyasaka, Y. Sakamoto, O. Terasaki: Dodecagonal tiling in mesoporous silica, Nature 487, 349–353 (2012)

    CAS  Google Scholar 

  • IZA-SC: Database of zeolite structures, http://asia.iza-structure.org/IZA-SC/ftc_table.php (2017)

  • M.W. Anderson, O. Terasaki, T. Ohsuna, A. Philippou, S. MacKay, A. Ferreira, J. Rocha, S. Lidin: Structure of the microporous titanosilicate ETS-10, Nature 367, 347–351 (1994)

    CAS  Google Scholar 

  • S. Nair, H.-K. Jeong, A. Chandrasekaran, C.M. Braunbarth, M. Tsapatsis, S.M. Kuznicki: Synthesis and structure determination of ETS-4 single crystals, Chem. Mater. 13, 4247–4254 (2001)

    CAS  Google Scholar 

  • J. Rocha, P. Brandao, Z. Lin, M.W. Anderson, V. Alfredsson, O. Terasaki: The first large-pore vanadosilicate framework containing hexacoordinated vanadium, Angew. Chem. Int. Ed. 36, 100–102 (1997)

    CAS  Google Scholar 

  • S.J. Datta, C. Khumnoon, Z.H. Lee, W.K. Moon, S. Docao, T.H. Nguyen, I.C. Hwang, D. Moon, P. Oleynikov, O. Terasaki, K.B. Yoon: CO2 capture from humid flue gases and humid atmosphere using a microporous coppersilicate, Science 350, 302–306 (2015)

    CAS  Google Scholar 

  • Z. Zhang, M. Sadakane, S.-I. Noro, N. Hiyoshi, A. Yoshida, M. Hara, W. Ueda: The assembly of an all-inorganic porous soft framework from metal oxide molecular nanowires, Chem. Eur. J. 23, 1972–1980 (2017)

    CAS  Google Scholar 

  • C.T. Kresge, M. Leonowicz, W. Roth, J.C. Vartuli, J. Beck: Ordered mesoporous molecular sieves synthesized by a liquid-crystal template mechanism, Nature 359, 710–712 (1992)

    CAS  Google Scholar 

  • Q. Huo, D.I. Margolese, U. Ciesla, D.G. Demuth, P. Feng, T.E. Gier, D.P. Siegel, A. Firouzi, B.F. Chmelka: Organization of organic molecules with inorganic molecular species into nanocomposite biphase arrays, Chem. Mater. 6, 1176–1191 (1994)

    CAS  Google Scholar 

  • Y. Wan, D. Zhao: On the controllable soft-templating approach to mesoporous silicates, Chem. Rev. 107, 2821–2860 (2007)

    CAS  Google Scholar 

  • J.N. Israelachvili, D.J. Mitchell, B.W. Ninham: Theory of self-assembly of hydrocarbon amphiphiles into micelles and bilayers, J. Chem. Soc. Faraday Trans. II 72, 1525–1568 (1976)

    CAS  Google Scholar 

  • H. Li, M. Eddaoudi, M. O'Keeffe, O.M. Yaghi: Design and synthesis of an exceptionally stable and highly porous metal-organic framework, Nature 402, 276–279 (1999)

    CAS  Google Scholar 

  • K.S. Park, Z. Ni, A.P. Côté, J.Y. Choi, R. Huang, F.J. Uribe-Romo, H.K. Chae, M.A. O'Keeffe, O.M. Yaghi: Exceptional chemical and thermal stability of zeolitic imidazolate frameworks, Proc. Natl. Acad. Sci. U.S.A. 103, 10186–10191 (2006)

    CAS  Google Scholar 

  • H.M. El-Kaderi, J.R. Hunt, J.L. Mendoza-Cortes, A.P. Côté, R.E. Taylor, M.A. O'Keeffe, O.M. Yaghi: Designed synthesis of 3-D covalent organic frameworks, Science 316, 268–272 (2007)

    CAS  Google Scholar 

  • P.M. Arnal, M. Comotti, F. Schüth: High-temperature-stable catalysts by hollow sphere encapsulation, Angew. Chem. Int. Ed. 45, 8224–8227 (2006)

    CAS  Google Scholar 

  • C. Galeano, R. Güttel, M. Paul, P. Arnal, A.-H. Lu, F. Schüth: Yolk-shell gold nanoparticles as model materials for support-effect studies in heterogeneous catalysis: Au, @C and Au, @ZrO2 for CO oxidation as an example, Chem. Eur. J. 17, 8434–8439 (2011)

    CAS  Google Scholar 

  • H.J. Shin, R. Ryoo, Z. Liu, O. Terasaki: Template synthesis of asymmetrically mesostructured platinum networks, J. Am. Chem. Soc. 123, 1246–1247 (2001)

    CAS  Google Scholar 

  • Z. Ma, T. Kyotani, Z. Liu, O. Terasaki, A. Tomita: Very high surface area microporous carbon with a three-dimensional nano-array structure: Synthesis and its molecular structure, Chem. Mater. 13, 4413–4415 (2001)

    CAS  Google Scholar 

  • K. Kim, T. Lee, Y. Kwon, Y. Seo, J. Song, J.K. Park, H. Lee, J.Y. Park, H. Ihee, S.J. Cho, R. Ryoo: Lanthanum-catalysed synthesis of microporous 3-D graphene-like carbons in a zeolite template, Nature 535, 131–135 (2016)

    CAS  Google Scholar 

  • J.W. Menter: The direct study by electron microscopy of crystal lattices and their imperfections, Proc. R. Soc. A 236, 119–135 (1956)

    CAS  Google Scholar 

  • J.W. Menter: The electron microscopy of crystal lattices, Adv. Phys. 7, 299–348 (1958)

    CAS  Google Scholar 

  • J.G. Allpress, J.V. Sanders: The direct observation of the structure of real crystals by lattice imaging, J. Appl. Crystallogr. 6, 165–190 (1973)

    CAS  Google Scholar 

  • M.A. O'Keeffe, J.V. Sanders: Phase-contrast component of lattice images of a zeolite crystal, Optik 46, 421–430 (1976)

    Google Scholar 

  • L.A. Bursill, E.A. Lodge, J.M. Thomas: Zeolitic structures as revealed by high-resolution electron microscopy, Nature 286, 111–113 (1980)

    CAS  Google Scholar 

  • L.A. Bursill, J.M. Thomas: High-resolution electron microscopy of microcrystalline partially crystalline and amorphous silicates, J. Phys. Chem. 85, 3007–3010 (1981)

    CAS  Google Scholar 

  • L.A. Bursill, J.M. Thomas, K.-J. Rao: Stability of zeolites under electron irradiation and imaging of heavy cations in silicates, Nature 289, 157–158 (1981)

    CAS  Google Scholar 

  • J.M. Thomas, G.R. Millward: Direct, real-space determination of intergrowths in ZSM-5/ZSM-11 catalysts, J. Chem. Soc. Chem. Commun. (1982), https://doi.org/10.1039/C39820001380

    Article  Google Scholar 

  • J.M. Thomas, G.R. Millward, L.A. Bursill: The ultrastructure of carbons, catalytically active graphitic compounds and zeolitic catalysts, Philos. Trans. R. Soc. A 300, 43–49 (1981)

    CAS  Google Scholar 

  • O. Terasaki, T. Ohsuna: TEM study on zeolite fine structures: Homework from Cambridge days, Top. Catal. 24, 13–18 (2003)

    CAS  Google Scholar 

  • O. Terasaki, J.M. Thomas: Imaging the structures of zeolite L and synthetic mazzite, Proc. R. Soc. A 395, 153–164 (1984)

    CAS  Google Scholar 

  • G.R. Millward, J.M. Thomas, O. Terasaki, D. Watanabe: Direct imaging and characterization of intergrowth-defects in erionite, Zeolites 6, 91–95 (1986)

    CAS  Google Scholar 

  • M.W. Anderson, K.S. Pachis, F.O. Prbin, S.W. Carr, O. Terasaki, T. Ohsuna, V. Alfreddson: Intergrowths of cubic and hexagonal polytypes of faujasitic zeolites, J. Chem. Soc. Chem. Commun. (1991), https://doi.org/10.1039/C39910001660

    Article  Google Scholar 

  • T. Ohsuna, O. Terasaki, Y. Nakagawa, S.I. Zones, K. Hiraga: Electron microscopic study of intergrowth of MFI and MEL: Crystal faults in B-MEL, J. Phys. Chem. B 101, 9881–9885 (1997)

    CAS  Google Scholar 

  • O. Terasaki, K. Yamazaki, J.M. Thomas, T. Ohsuna, D. Watanabe, J.V. Sanders, J.C. Barry: Isolating individual chains of selenium by incorporation into the channels of a zeolite, Nature 330, 58–60 (1987)

    CAS  Google Scholar 

  • J.-O. Bovin, V. Alfredsson, G. Karlsson, A. Carlsson, Z. Blum, O. Terasaki: TEM-tomography of FAU-zeolite crystals containing Pt-clusters, Ultramicroscopy 62, 277–281 (1996)

    CAS  Google Scholar 

  • O. Terasaki, Z.K. Tang, Y. Nozue, T. Goto: PbI2 confined in the spaces of LTA zeolites, MRS Proceedings 233, 139 (1991)

    CAS  Google Scholar 

  • A. Carlsson, T. Oku, J.O. Bovin, G. Karlsson, Y. Okamoto, N. Ohnishi, O. Terasaki: The structure of iron oxide implanted zeolite Y, determined by high-resolution electron microscopy and refined with selected area electron diffraction amplitudes, Chem. Eur. J. 5, 244–249 (1999)

    CAS  Google Scholar 

  • Y. Sakamoto, N. Togashi, O. Terasaki, T. Ohsuna, Y. Okamoto, K. Hiraga: MoS2 clusters in the spaces of FAU zeolite, Mater. Sci. Eng. A 217/218, 147–150 (1996)

    Google Scholar 

  • P. Wagner, O. Terasaki, S. Ritsch, J.G. Nery, S.I. Zones, M.E. Davis, K. Hiraga: Electron diffraction structure solution of a nanocrystalline zeolite at atomic resolution, J. Phys. Chem. B 103, 8245–8250 (1999)

    CAS  Google Scholar 

  • Z. Liu, T. Ohsuna, O. Terasaki, M.A. Camblor, M.J. Diaz-Cabañas, K. Hiraga: The first zeolite with three-dimensional intersecting straight-channel system of 12-membered rings, J. Am. Chem. Soc. 123, 5370–5371 (2001)

    CAS  Google Scholar 

  • T. Ohsuna, Z. Liu, O. Terasaki, K. Hiraga, M. Camblor: Framework determination of a polytype of zeolite beta by using electron crystallography, J. Phys. Chem. B 106, 5673–5678 (2002)

    CAS  Google Scholar 

  • T. Ohsuna, O. Terasaki, D. Watanabe, M.W. Anderson, S.W. Carr: Dealumination of hexagonal (EMT)/cubic (FAU) zeolite intergrowth materials: A SEM and HRTEM study, Chem. Mater. 6, 2201–2204 (1994)

    CAS  Google Scholar 

  • S. Inagaki, S. Guan, T. Ohsuna, O. Terasaki: An ordered mesoporous organosilica hybrid material with a crystal-like wall structure, Nature 416, 304–307 (2002)

    CAS  Google Scholar 

  • O. Terasaki: Electron microscopy studies in molecular sieve science. In: Structures and Structure Determination, ed. by H.G. Karge, J. Weitkamp (Springer, Berlin, Heidelberg 1999) pp. 71–112

    Google Scholar 

  • O. Terasaki, T. Ohsuna: Structural study of microporous and mesoporous materials by transmission electron microscopy. In: Handbook of Zeolite Science and Technology, ed. by S.M. Auerbach, K.A. Carrado, P.K. Dutta (CRC, Boca Raton 2003)

    Google Scholar 

  • O. Terasaki, T. Ohsuna: Is electron microscope an efficient magnifying glass for micro- and meso-porous materials? In: Proc. 13th Int. Zeolite Conf (Elsevier, Amsterdam 2001) pp. 61–71

    Google Scholar 

  • O. Terasaki, T. Ohsuna, Z. Liu, M. Kaneda, S. Kamiya, A. Carlsson, T. Tsubakiyama, Y. Sakamoto, S. Inagaki, S. Che, T. Tatsumi, M.A. Camblor, R. Ryoo, D. Zhao, G. Stucky, D. Shindo, K. Hiraga: Porous Materials: Looking Through the Electron Microscope (Elsevier, Amsterdam 2002)

    Google Scholar 

  • I. Díaz, A. Mayoral: TEM studies of zeolites and ordered mesoporous materials, Micron 42, 512–527 (2011)

    Google Scholar 

  • A. Mayoral, R. Arenal, V. Gascón, C. Márquez-Álvarez, R.M. Blanco, I. Díaz: Designing functionalized mesoporous materials for enzyme immobilization: Locating enzymes by using advanced TEM techniques, ChemCatChem 5, 903–909 (2013)

    CAS  Google Scholar 

  • D. Denysenko, M. Grzywa, M. Tonigold, B. Streppel, I. Krkljus, M. Hirscher, E. Mugnaioli, U. Kolb, J. Hanss, D. Volkmer: Elucidating gating effects for hydrogen sorption in MFU-4-type triazolate-based metal-organic frameworks featuring different pore sizes, Chem. Eur. J. 17, 1837–1848 (2011)

    CAS  Google Scholar 

  • M. Feyand, E. Mugnaioli, F. Vermoortele, B. Bueken, J.M. Dieterich, T. Reimer, U. Kolb, D. de Vos, N. Stock: Automated diffraction tomography for the structure elucidation of twinned, sub-micrometer crystals of a highly porous, catalytically active bismuth metal-organic framework, Angew. Chem. Int. Ed. 51, 10373–10376 (2012)

    CAS  Google Scholar 

  • E. Mugnaioli, U. Kolb: Applications of automated diffraction tomography (ADT) on nanocrystalline porous materials, Microporous Mesoporous Mater. 166, 93–101 (2013)

    CAS  Google Scholar 

  • Y. Yun, W. Wan, F. Rabbani, J. Su, H. Xu, S. Hovmöller, M. Johnsson, X. Zou: Phase identification and structure determination from multiphase crystalline powder samples by rotation electron diffraction, J. Appl. Crystallogr. 47, 2048–2054 (2014)

    CAS  Google Scholar 

  • O.I. Lebedev, F. Millange, C. Serre, G. van Tendeloo, G. Férey: First direct imaging of giant pores of the metal-organic framework MIL-101, Chem. Mater. 17, 6525–6527 (2005)

    CAS  Google Scholar 

  • C. Wiktor, S. Turner, D. Zacher, R.A. Fischer, G. van Tendeloo: Imaging of intact MOF-5 nanocrystals by advanced TEM at liquid nitrogen temperature, Microporous Mesoporous Mater. 162, 131–135 (2012)

    CAS  Google Scholar 

  • L. Zhu, D. Zhang, M. Xue, H. Li, S. Qiu: Direct observations of the MOF (UiO-66) structure by transmission electron microscopy, CrystEngComm 15, 9356–9359 (2013)

    CAS  Google Scholar 

  • J. Cravillon, S. Muenzer, S.-J. Lohmeier, A. Feldhoff, K. Huber, M. Wiebcke: Rapid room-temperature synthesis and characterization of nanocrystals of a prototypical zeolitic imidazolate framework, Chem. Mater. 21, 1410–1412 (2009)

    CAS  Google Scholar 

  • A. Mayoral: Atomic resolution analysis of porous solids: A detailed study of silver ion-exchanged zeolite A, Microporous Mesoporous Mater. 166, 117–122 (2013)

    CAS  Google Scholar 

  • A. Mayoral, J. Coronas, C. Casado, C. Tellez, I. Díaz: Atomic resolution analysis of microporous titanosilicate ETS-10 through aberration corrected STEM imaging, ChemCatChem 5, 2595–2598 (2013)

    CAS  Google Scholar 

  • A. Mayoral, P.A. Anderson, I. Díaz: Zeolites are no longer a challenge: Atomic resolution data by aberration-corrected STEM, Micron 68, 146–151 (2015)

    CAS  Google Scholar 

  • A. Mayoral, T. Carey, P.A. Anderson, A. Lubk, I. Díaz: Atomic resolution analysis of silver ion-exchanged zeolite A, Angew. Chem. Int. Ed. 50, 11230–11233 (2011)

    CAS  Google Scholar 

  • A. Mayoral, J.E. Readman, P.A. Anderson: Aberration-corrected STEM analysis of a cubic Cd array encapsulated in zeolite A, J. Phys. Chem. C 117, 24485–24489 (2013)

    CAS  Google Scholar 

  • A.E. Garcia-Bennett, N. Kupferschmidt, Y. Sakamoto, S. Che, O. Terasaki: Synthesis of mesocage structures by kinetic control of self-assembly in anionic surfactants, Angew. Chem. Int. Ed. 44, 5317–5322 (2005)

    CAS  Google Scholar 

  • M. Choi, K. Na, J. Kim, Y. Sakamoto, O. Terasaki, R. Ryoo: Stable single-unit-cell nanosheets of zeolite MFI as active and long-lived catalysts, Nature 461, 246–249 (2009)

    CAS  Google Scholar 

  • K. Lund, N. Muroyama, O. Terasaki: Accidental extinction in powder XRD intensity of porous crystals: Mesoporous carbon crystal CMK-5 and layered zeolite-nanosheets, Microporous Mesoporous Mater. 128, 71–77 (2010)

    CAS  Google Scholar 

  • L. Han, K. Miyasaka, O. Terasaki: Electron crystallography. In: Structure from Diffraction Methods, ed. by D.W. Bruce, D. O'Hare, R.I. Walton (Wiley, Chichester 2014) pp. 201–258

    Google Scholar 

  • J.M. Zuo, J.C.H. Spence: Electron Microdiffraction (Springer, New York 2013)

    Google Scholar 

  • D. Watanabe, R. Uyeda, A. Fukuhara: Determination of the atom form factor by high-voltage electron diffraction, Acta Crystallogr. A 25, 138–140 (1969)

    CAS  Google Scholar 

  • M. Fujimoto, O. Terasaki, D. Watanabe: Determination of atomic scattering factors of vanadium and chromium by means of vanishing Kikuchi line method, Phys. Lett. A 41, 159–160 (1972)

    CAS  Google Scholar 

  • P.A. Doyle, P.S. Turner: Relativistic Hartree-Fock x-ray and electron scattering factors, Acta Crystallogr. A 24, 390–397 (1968)

    CAS  Google Scholar 

  • Z. Liu, N. Fujita, K. Miyasaka, L. Han, S.M. Stevens, M. Suga, S. Asahina, B. Slater, C. Xiao, Y. Sakamoto, M.W. Anderson, R. Ryoo, O. Terasaki: A review of fine structures of nanoporous materials as evidenced by microscopic methods, J. Electron Microsc. 62, 109–146 (2013)

    CAS  Google Scholar 

  • D. Watanabe, O. Terasaki: Experimental study on the ionicity in the TiO phase. An application of the new method of determining the structure factor by high voltage electron diffraction. In: Solid State Chemistry, NBS Special Publication, Vol. 364, ed. by R.S. Roth, S.J. Schneider (U.S. Govt. Printing Office, Washington D.C. 1972) pp. 155–164

    Google Scholar 

  • T. Arii, R. Uyeda, O. Terasaki, D. Watanabe: Accurate determination of atomic scattering factors of f.c.c. and h.c.p. metals by high-voltage electron diffraction, Acta Crystallogr. A 29, 295–298 (1973)

    CAS  Google Scholar 

  • O. Terasaki, T. Fukamachi, S. Hosoya, D. Watanabe: Anisotropy of Compton profile on vanadium single crystal, Phys. Lett. A 43, 123–124 (1973)

    CAS  Google Scholar 

  • S. Ohara, T. Fukamachi, S. Hosoya, T. Takeda, O. Terasaki: Anisotropy of Compton profile on chromium single crystal, Phys. Lett. A 49, 337–338 (1974)

    Google Scholar 

  • J.M. Zuo, M. Kim, M. O'Keeffe, J.C.H. Spence: Direct observation of d-orbital holes and Cu--Cu bonding in Cu2O, Nature 401, 49–52 (1999)

    CAS  Google Scholar 

  • K. Tsuda, Y. Ogata, K. Takagi, T. Hashimoto, M. Tanaka: Refinement of crystal structural parameters and charge density using convergent-beam electron diffraction---The rhombohedral phase of LaCrO3, Acta Crystallogr. A 58, 514–525 (2002)

    Google Scholar 

  • B.K. Vainshtein: Fundamentals of Crystals. Symmetry and Methods of Structural Crystallography, Modern Crystallography, Vol. 1 (Springer, Heidelberg 1994)

    Google Scholar 

  • L. Palatinus, P. Brázda, P. Boullay, O. Perez, M. Klementová, S. Petit, V. Eigner, M. Zaarour, S. Mintova: Hydrogen positions in single nanocrystals revealed by electron diffraction, Science 355, 166–169 (2017)

    CAS  Google Scholar 

  • R. Vincent, P.A. Midgley: Double conical beam-rocking system for measurement of integrated electron diffraction intensities, Ultramicroscopy 53, 271–282 (1994)

    CAS  Google Scholar 

  • U. Kolb, T. Gorelik, C. Kübel, M.T. Otten, D. Hubert: Towards automated diffraction tomography: Part I---Data acquisition, Ultramicroscopy 107, 507–513 (2007)

    CAS  Google Scholar 

  • U. Kolb, T. Gorelik, M.T. Otten: Towards automated diffraction tomography. Part II---Cell parameter determination, Ultramicroscopy 108, 763–772 (2008)

    CAS  Google Scholar 

  • D. Zhang, P. Oleynikov, S. Hovmöller, X. Zou: Collecting 3-D electron diffraction data by the rotation method, Z. Kristallogr. 225, 94–102 (2010)

    CAS  Google Scholar 

  • M. Gemmi, P. Oleynikov: Scanning reciprocal space for solving unknown structures: Energy filtered diffraction tomography and rotation diffraction tomography methods, Z. Kristallogr. 228, 51–58 (2013)

    CAS  Google Scholar 

  • X. Zou, S. Hovmöller, P. Oleynikov: Electron Crystallography: Electron Microscopy and Electron Diffraction (Oxford Univ. Press, Oxford 2011)

    Google Scholar 

  • T.E. Gorelik, A.A. Stewart, U. Kolb: Structure solution with automated electron diffraction tomography data: Different instrumental approaches, J. Microsc. 244, 325–331 (2011)

    CAS  Google Scholar 

  • EDT 3-D: AnaliteX, http://www.edt3d.com

  • NanoMEGAS: DigiStar Precession Unit, http://www.nanomegas.com

  • TVIPS GmbH: Universal Scan Generator, https://www.tvips.com/accessories/universal-scan-generator/

  • M. Gemmi, M.G.I. La Placa, A.S. Galanis, E.F. Rauch, S. Nicolopoulos: Fast electron diffraction tomography, J. Appl. Crystallogr. 48, 718–727 (2015)

    CAS  Google Scholar 

  • D. Shi, B.L. Nannenga, M.G. Iadanza, T. Gonen: Three-dimensional electron crystallography of protein microcrystals, eLIFE 2, e01345 (2013)

    Google Scholar 

  • S. Schlitt, T.E. Gorelik, A.A. Stewart, E. Schömer, T. Raasch, U. Kolb: Application of clustering techniques to electron-diffraction data: Determination of unit-cell parameters, Acta Crystallogr. A 68, 536–546 (2012)

    CAS  Google Scholar 

  • T.E. Gorelik, J. van de Streek, A.F.M. Kilbinger, G. Brunklaus, U. Kolb: Ab-initio crystal structure analysis and refinement approaches of oligo p-benzamides based on electron diffraction data, Acta Crystallogr. B 68, 171–181 (2012)

    CAS  Google Scholar 

  • I. Rozhdestvenskaya, E. Mugnaioli, M. Czank: The structure of charoite, (K,Sr,Ba,Mn)15--16(Ca,Na)32[(Si70(O,OH)180)](OH,F)4.0·nH2O, solved by conventional and automated electron diffraction, Mineral. Mag. 74, 159–177 (2010)

    CAS  Google Scholar 

  • E. Mugnaioli, I. Andrusenko, T. Schüler, N. Loges, R.E. Dinnebier, M. Panthöfer, W. Tremel, U. Kolb: Ab initio structure determination of vaterite by automated electron diffraction, Angew. Chem. Int. Ed. 51, 7041–7045 (2012)

    CAS  Google Scholar 

  • J. Jiang, J.L. Jordá, J. Yu, L.A. Baumes, E. Mugnaioli, M.J. Díaz-Cabañas, U. Kolb, A. Corma: Synthesis and structure determination of the hierarchical meso-microporous zeolite ITQ-43, Science 333, 1131–1134 (2011)

    CAS  Google Scholar 

  • G. Bellussi, E. Montanari, E. Di Paola, R. Millini, A. Carati, C. Rizzo, W.O.J. Parker, M. Gemmi, E. Mugnaioli, U. Kolb, S. Zanardi: ECS-3: A crystalline hybrid organic-inorganic aluminosilicate with open porosity, Angew. Chem. Int. Ed. 51, 666–669 (2012)

    CAS  Google Scholar 

  • I. Andrusenko, E. Mugnaioli, T.E. Gorelik, D. Koll, M. Panthöfer, W. Tremel, U. Kolb: Structure analysis of titanate nanorods by automated electron diffraction tomography, Acta Crystallogr. B 67, 218–225 (2011)

    CAS  Google Scholar 

  • T. Willhammar, J. Sun, W. Wan, P. Oleynikov, D. Zhang, X. Zou, M. Moliner, J. Gonzalez, C. Martínez, F. Rey, A. Corma: Structure and catalytic properties of the most complex intergrown zeolite ITQ-39 determined by electron crystallography, Nat. Chem. 4, 188 (2012)

    CAS  Google Scholar 

  • Y. Li, L. Zhang, A. Torres-Pardo, J.M. Gonzalez-Calbet, Y. Ma, P. Oleynikov, O. Terasaki, S. Asahina, M. Shima, D. Cha, L. Zhao, K. Takanabe, J. Kubota, K. Domen: Cobalt phosphate-modified barium-doped tantalum nitride nanorod photoanode with 1.5% solar energy conversion efficiency, Nat. Commun. 4, 2566 (2013)

    Google Scholar 

  • A. Mayence, J.R.G. Navarro, Y. Ma, O. Terasaki, L. Bergström, P. Oleynikov: Phase identification and structure solution by three-dimensional electron diffraction tomography: Gd-phosphate nanorods, Inorg. Chem. 53, 5067–5072 (2014)

    CAS  Google Scholar 

  • J.R.G. Navarro, A. Mayence, J. Andrade, F. Lerouge, F. Chaput, P. Oleynikov, L. Bergström, S. Parola, A. Pawlicka: WO3 nanorods created by self-assembly of highly crystalline nanowires under hydrothermal conditions, Langmuir 30, 10487–10492 (2014)

    CAS  Google Scholar 

  • M. Zhong, Y. Ma, P. Oleynikov, K. Domen, J.-J. Delaunay: A conductive ZnO–ZnGaON nanowire-array-on-a-film photoanode for stable and efficient sunlight water splitting, Energy Environ. Sci. 7, 1693–1699 (2014)

    CAS  Google Scholar 

  • A. Mayence, D. Wang, G. Salazar-Alvarez, P. Oleynikov, L. Bergström: Probing planar defects in nanoparticle superlattices by 3-D small-angle electron diffraction tomography and real space imaging, Nanoscale 6, 13803–13808 (2014)

    CAS  Google Scholar 

  • Q. Sun, Y. Ma, N. Wang, X. Li, D. Xi, J. Xu, F. Deng, K.B. Yoon, P. Oleynikov, O. Terasaki, J. Yu: High performance nanosheet like silicoaluminophosphate molecular sieves: Synthesis, 3-D EDT structural analysis and MTO catalytic studies, J. Mater. Chem. A 2, 17828–17839 (2014)

    CAS  Google Scholar 

  • Y. Liu, Y. Ma, Y. Zhao, X. Sun, F. Gándara, H. Furukawa, Z. Liu, H. Zhu, C. Zhu, K. Suenaga, P. Oleynikov, A.S. Alshammari, X. Zhang, O. Terasaki, O.M. Yaghi: Weaving of organic threads into a crystalline covalent organic framework, Science 351, 365–369 (2016)

    CAS  Google Scholar 

  • Y. Ma, P. Oleynikov, O. Terasaki: Electron crystallography for determining the handedness of a chiral zeolite nanocrystal, Nat. Mater. 16, 755–759 (2017)

    CAS  Google Scholar 

  • P. Mooney: Optimization of image collection for cellular electron microscopy, Methods Cell Biol. 79, 661–719 (2007)

    Google Scholar 

  • M. Pan: Direct detection and electron counting—A beginning of a new era for electron microscopy. In: Proc. 16th Eur. Microsc. Congr., Lyon (2017)

    Google Scholar 

  • X. Li, S.Q. Zheng, K. Egami, D.A. Agard, Y. Cheng: Influence of electron dose rate on electron counting images recorded with the K2 camera, J. Structural Biol. 184, 251–260 (2013)

    CAS  Google Scholar 

  • M.W. Tate, P. Purohit, D. Chamberlain, K.X. Nguyen, R. Hovden, C.S. Chang, P. Deb, E. Turgut, J.T. Heron, D.G. Schlom, D.C. Ralph, G.D. Fuchs, K.S. Shanks, H.T. Philipp, D.A. Muller, S.M. Gruner: High dynamic range pixel array detector for scanning transmission electron microscopy, Microsc. Microanal. 22, 237–249 (2016)

    CAS  Google Scholar 

  • H. Ryll, M. Simson, R. Hartmann, P. Holl, M. Huth, S. Ihle, Y. Kondo, P. Kotula, A. Liebel, K. Müller-Caspary, A. Rosenauer, R. Sagawa, J. Schmidt, H. Soltau, L. Strüder: A pnCCD-based, fast direct single electron imaging camera for TEM and STEM, J. Instrum. 11, P04006 (2016)

    Google Scholar 

  • A. Mayoral, L.F. Allard, D. Ferrer, R. Esparza, M. Jose-Yacaman: On the behavior of Ag nanowires under high temperature: In situ characterization by aberration-corrected STEM, J. Mater. Chem. 21, 893–898 (2011)

    CAS  Google Scholar 

  • M.M. Mariscal, A. Mayoral, J.A. Olmos-Asar, C. Magen: Nanoalloying in real time. A high resolution STEM and computer simulation study, Nanoscale 3, 5013–5019 (2011)

    CAS  Google Scholar 

  • M. Adrian, J. Dubochet, J. Lepault, A.W. McDowall: Cryo-electron microscopy of viruses, Nature 308, 32–36 (1984)

    CAS  Google Scholar 

  • M. Hÿtch, F. Houdellier, F. Hüe, E. Snoeck: Nanoscale holographic interferometry for strain measurements in electronic devices, Nature 453, 1086–1089 (2008)

    Google Scholar 

  • N. De Jonge, F.M. Ross: Electron microscopy of specimens in liquid, Nat. Nanotechnol. 6, 695–704 (2011)

    Google Scholar 

  • H.-G. Liao, L. Cui, S. Whitelam, H. Zheng: Real-time imaging of Pt3Fe nanorod growth in solution, Science 336, 1011–1014 (2012)

    CAS  Google Scholar 

  • K.L. Jungjohann, S. Bliznakov, P.W. Sutter, E.A. Stach, E.A. Sutter: In situ liquid cell electron microscopy of the solution growth of Au--Pd core--shell nanostructures, Nano Lett. 13, 2964–2970 (2013)

    CAS  Google Scholar 

  • J.E. Evans, K.L. Jungjohann, N.D. Browning, I. Arslan: Controlled growth of nanoparticles from solution with in situ liquid transmission electron microscopy, Nano Lett. 11, 2809–2813 (2011)

    CAS  Google Scholar 

  • T.J. Woehl, C. Park, J.E. Evans, I. Arslan, W.D. Ristenpart, N.D. Browning: Direct observation of aggregative nanoparticle growth: Kinetic modeling of the size distribution and growth rate, Nano Lett. 14, 373–378 (2014)

    CAS  Google Scholar 

  • H. Deng, S. Grunder, K.E. Cordova, C. Valente, H. Furukawa, M. Hmadeh, F. Gándara, A.C. Whalley, Z. Liu, S. Asahina, H. Kazumori, M.A. O'Keeffe, O. Terasaki, J.F. Stoddart, O.M. Yaghi: Large-pore apertures in a series of metal-organic frameworks, Science 336, 1018–1023 (2012)

    CAS  Google Scholar 

  • S. Ogawa, D. Watanabe: Crosses observed in the electron-diffraction pattern of an orientated CuAu film, Acta Crystallogr. 5, 848–849 (1952)

    CAS  Google Scholar 

  • S. Ogawa, D. Watanabe: On the structure of CuAu II revealed by electron diffraction, Acta Crystallogr. 7, 377–378 (1954)

    CAS  Google Scholar 

  • J.M. Cowley: Structure analysis of single crystals by electron diffraction. I. Techniques, Acta Crystallogr. 6, 516–521 (1953)

    CAS  Google Scholar 

  • S. Kuwabara: Accurate determination of hydrogen positions in NH4Cl by electron diffraction, J. Phys. Soc. Jpn. 14, 1205–1216 (1959)

    CAS  Google Scholar 

  • D.L. Dorset, H.A. Hauptman: Direct phase determination for quasi-kinematical electron diffraction intensity data from organic microcrystals, Ultramicroscopy 1, 195–201 (1976)

    CAS  Google Scholar 

  • D.L. Dorset, C.J. Gilmore: Ab initio electron diffraction structure analysis of zeolites -- Direct methods determination of NaY, Z. Kristallogr. 226, 447–453 (2011)

    CAS  Google Scholar 

  • N. Ohnishi, T. Ohsuna, Y. Sakamoto, O. Terasaki, K. Hiraga: Quantitative HRTEM study of zeolite, Microporous Mesoporous Mater. 21, 581–588 (1998)

    CAS  Google Scholar 

  • C. Baerlocher, A. Hepp, W.M. Meier: DLS-76: Distance least-squares refinement program, ETH Zürich, www.crystal.mat.ethz.ch/software/index.html (1977)

  • D.L. Dorset, S.C. Weston, S.S. Dhingra: Crystal structure of zeolite MCM-68: A new three-dimensional framework with large pores, J. Phys. Chem. B 110, 2045–2050 (2006)

    CAS  Google Scholar 

  • D.L. Dorset: The crystal structure of ZSM-10, a powder x-ray and electron diffraction study, Z. Kristallogr. 221, 260–265 (2006)

    CAS  Google Scholar 

  • T. Conradsson, M.S. Dadachov, X.D. Zou: Synthesis and structure of (Me3N)6[Ge32O64]\(\cdot\)(H2O)4.5, a thermally stable novel zeotype with 3-D interconnected 12-ring channels, Microporous Mesoporous Mater. 41, 183–191 (2000)

    CAS  Google Scholar 

  • B. Slater, C.R.A. Catlow, Z. Liu, T. Ohsuna, O. Terasaki, M.A. Camblor: Surface structure and crystal growth of zeolite Beta C, Angew. Chem. Int. Ed. 41, 1235–1237 (2002)

    CAS  Google Scholar 

  • B. Slater, T. Ohsuna, Z. Liu, O. Terasaki: Insights into the crystal growth mechanisms of zeolites from combined experimental imaging and theoretical studies, Faraday Discuss. 136, 125–141 (2007)

    CAS  Google Scholar 

  • L. Han, T. Ohsuna, Z. Liu, V. Alfredsson, T. Kjellman, S. Asahina, M. Suga, Y. Ma, P. Oleynikov, K. Miyasaka, A. Mayoral, I. Díaz, Y. Sakamoto, S.M. Stevens, M.W. Anderson, C. Xiao, N. Fujita, A.E. Garcia-Bennett, K.B. Yoon, S. Che, O. Terasaki: Silica-based nanoporous materials, Z. Anorg. Allg. Chem. 640, 521–536 (2014)

    CAS  Google Scholar 

  • V. Alfredsson, T. Ohsuna, O. Terasaki, J.-O. Bovin: Investigation of the surface structure of the zeolites FAU and EMT by high-resolution transmission electron microscopy, Angew. Chem. Int. Ed. 32, 1210–1213 (1993)

    Google Scholar 

  • M. Taramasso, G. Perego, B. Notari: Preparation of porous crystalline synthetic materials comprised of silicon and titanium oxides, US Patent 4410501 (1983)

    Google Scholar 

  • X. Wang, A.J. Jacobson: Crystal structure of the microporous titanosilicate ETS-10 refined from single crystal x-ray diffraction data, Chem. Commun. (1999), https://doi.org/10.1039/A901280J

    Article  Google Scholar 

  • M.W. Anderson, J.R. Agger, D.-P. Luigi, A.K. Baggaley, J. Rocha: Cation sites in ETS-10: 23Na 3Q MAS NMR and lattice energy minimisation calculations, Phys. Chem. Chem. Phys. 1, 2287–2292 (1999)

    CAS  Google Scholar 

  • M.E. Grillo, J. Carrazza: Computational modeling of the nonframework cation location and distribution in microporous titanosilicate ETS-10, J. Phys. Chem. 100, 12261–12264 (1996)

    CAS  Google Scholar 

  • A. Damin, F.X. Llabrés i Xamena, C. Lamberti, B. Civalleri, C.M. Zicovich-Wilson, A.A. Zecchina: Structural, electronic, and vibrational properties of the Ti–O–Ti quantum wires in the titanosilicate ETS-10, J. Phys. Chem. B 108, 1328–1336 (2003)

    Google Scholar 

  • M. Koç, S. Galioglu, D. Toffoli, H. Üstünel, B. Akata: Understanding the effects of ion-exchange in titanosilicate ETS-10: A joint theoretical and experimental study, J. Phys. Chem. C 118, 27281–27291 (2014)

    Google Scholar 

  • A. Mayoral, R.M. Hall, R. Jackowska, J.E. Readman: Imaging the atomic position of light cations in a porous network and the europium(III) ion exchange capability by aberration-corrected electron microscopy, Angew. Chem. Int. Ed. 55, 16127–16131 (2016)

    CAS  Google Scholar 

  • M.W. Anderson, O. Terasaki, T. Ohsuna, P.J.O. Malley, A. Philippou, S.P. Mackay, A. Ferreira, J. Rocha, S. Lidin: Microporous titanosilicate ETS-10: A structural survey, Philos. Mag. B 71, 813–841 (1995)

    CAS  Google Scholar 

  • C. Casado, Z. Amghouz, J.R. García, K. Boulahya, J.M. Gonzalez-Calbet, C. Tellez, J. Coronas: Synthesis and characterization of microporous titanosilicate ETS-10 obtained with different Ti sources, Mater. Res. Bull. 44, 1225–1231 (2009)

    CAS  Google Scholar 

  • W.Y. Ching, Y.N. Xu, Z.Q. Gu: Structure and properties of microporous titanosilicate determined by first-principles calculations, Phys. Rev. B 54, R15585–R15589 (1996)

    CAS  Google Scholar 

  • J. Rocha, A. Ferreira, Z. Lin, M.W. Anderson: Synthesis of microporous titanosilicate ETS-10 from TiCl3 and TiO2: A comprehensive study, Microporous Mesoporous Mater. 23, 253–263 (1998)

    CAS  Google Scholar 

  • P.A. Midgley, A.S. Eggeman: Precession electron diffraction—A topical review, IUCrJ. 2, 126–136 (2015)

    CAS  Google Scholar 

  • P. Oleynikov, S. Hovmöller, X.D. Zou: Precession electron diffraction: Observed and calculated intensities, Ultramicroscopy 107, 523–533 (2007)

    CAS  Google Scholar 

  • D. Zhao, J. Feng, Q. Huo, N. Melosh, G.H. Fredrickson, B.F. Chmelka, G.D. Stucky: Triblock copolymer syntheses of mesoporous silica with periodic 50 to 300 angstrom pores, Science 279, 548 (1998)

    CAS  Google Scholar 

  • T. Kimura, T. Kamata, M. Fuziwara, Y. Takano: Formation of novel ordered mesoporous silicas with square channels and their direct observation by transmission electron microscopy, Angew. Chem. Int. Ed. 39, 3855–3859 (2000)

    CAS  Google Scholar 

  • S. Inagaki, S. Guan, Y. Fukushima, T. Ohsuna, O. Terasaki: Novel mesoporous materials with a uniform distribution of organic groups and inorganic oxide in their frameworks, J. Am. Chem. Soc. 121, 9611–9614 (1999)

    CAS  Google Scholar 

  • Y. Sakamoto, L. Han, S. Che, O. Terasaki: Structural analyses of intergrowth and stacking fault in cage-type mesoporous crystals, Chem. Mater. 21, 223–229 (2009)

    CAS  Google Scholar 

  • K. Miyasaka, L. Han, S. Che, O. Terasaki: A lesson from the unusual morphology of silica mesoporous crystals: Growth and close packing of spherical micelles with multiple twinning, Angew. Chem. Int. Ed. 45, 6516–6519 (2006)

    CAS  Google Scholar 

  • L. Han, Y. Sakamoto, O. Terasaki, Y. Li, S. Che: Synthesis of carboxylic group functionalized mesoporous silicas (CFMSs) with various structures, J. Mater. Chem. 17, 1216–1221 (2007)

    CAS  Google Scholar 

  • Y. Ma, L. Han, K. Miyasaka, P. Oleynikov, S. Che, O. Terasaki: Structural study of hexagonal close-packed silica mesoporous crystal, Chem. Mater. 25, 2184–2191 (2013)

    CAS  Google Scholar 

  • K. Miyasaka, A.G. Bennett, L. Han, Y. Han, C. Xiao, N. Fujita, T. Castle, Y. Sakamoto, S. Che, O. Terasaki: The role of curvature in silica mesoporous crystals, Interface Focus 2, 634–644 (2012)

    Google Scholar 

  • L. Han, Y. Sakamoto, S. Che, O. Terasaki: Insight into the defects of cage-type silica mesoporous crystals with Fd3m symmetry: TEM observations and a new proposal of ‘‘polyhedron packing'' for the crystals, Chem. Eur. J. 15, 2818–2825 (2009)

    CAS  Google Scholar 

  • E. Matzke: The three-dimensional shape of bubbles in foam---An analysis of the role of surface forces in three-dimensional cell shape determination, Am. J. Biol. 33, 58–80 (1946)

    CAS  Google Scholar 

  • Y. Sakamoto, O. Terasaki: A layer stacking with large repeating unit in multi-modal cage-type anionic-surfactant-templated silica mesoporous crystal, Solid State Sci. 13, 762–767 (2011)

    CAS  Google Scholar 

  • T. Ohsuna, Y. Sakamoto, O. Terasaki, K. Kuroda: TEM image simulation of mesoporous crystals for structure type identification, Solid State Sci. 13, 736–744 (2011)

    CAS  Google Scholar 

  • T. Dotera: Toward the discovery of new soft quasicrystals: From a numerical study viewpoint, J. Polym. Sci. B 50, 155–167 (2011)

    Google Scholar 

  • J.-F. Sadoc, R. Mosseri: Quasiperiodic Frank–Kasper phases derived from the square–triangle dodecagonal tiling, Struct. Chem. 28, 63–73 (2016)

    Google Scholar 

  • C. Gao, Y. Sakamoto, O. Terasaki, S. Che: Formation of diverse mesophases templated by a diprotic anionic surfactant, Chem. Eur. J. 14, 11423–11428 (2008)

    CAS  Google Scholar 

  • S.J. Cox, F. Graner, R. Mosseri, J.F. Sadoc: Quasicrystalline three-dimensional foams, J. Phys. Condens. Matter 29, 114001 (2017)

    CAS  Google Scholar 

  • T. Ohsuna, Z. Liu, S. Che, O. Terasaki: Characterization of chiral mesoporous materials by transmission electron microscopy, Small 1, 233–237 (2005)

    CAS  Google Scholar 

  • S. Che, Z. Liu, T. Ohsuna, K. Sakamoto, O. Terasaki, T. Tatsumi: Synthesis and characterization of chiral mesoporous silica, Nature 429, 281–284 (2004)

    CAS  Google Scholar 

  • K. Grosse-Brauckmann: Triply periodic minimal and constant mean curvature surfaces, Interface Focus 2, 582–588 (2012)

    Google Scholar 

  • S.T. Hyde, Z. Blum, T. Landh, S. Lidin, B.W. Ninham: The Language of Shape: The Role of Curvature in Condensed Matter: Physics, Chemistry and Biology (Elsevier, Amsterdam 1996)

    Google Scholar 

  • L. Han, K. Miyasaka, O. Terasaki, S. Che: Evolution of packing parameters in the structural changes of silica mesoporous crystals: Cage-type, 2-D cylindrical, bicontinuous diamond and gyroid, and lamellar, J. Am. Chem. Soc. 133, 11524–11533 (2011)

    CAS  Google Scholar 

  • L. Han, P. Xiong, J. Bai, S. Che: Spontaneous formation and characterization of silica mesoporous crystal spheres with reverse multiply twinned polyhedral hollows, J. Am. Chem. Soc. 133, 6106–6109 (2011)

    CAS  Google Scholar 

  • S.T. Hyde: Handbook of Applied Surface and Colloidal Chemistry (Wiley, Hoboken 2001)

    Google Scholar 

  • L. Han, D. Xu, Y. Liu, T. Ohsuna, Y. Yao, C. Jiang, Y. Mai, Y. Cao, Y. Duan, S. Che: Synthesis and characterization of macroporous photonic structure that consists of azimuthally shifted double-diamond silica frameworks, Chem. Mater. 26, 7020–7028 (2014)

    CAS  Google Scholar 

  • X. Cao, D. Xu, Y. Yao, L. Han, O. Terasaki, S. Che: Interconversion of triply periodic constant mean curvature surface structures: From double diamond to single gyroid, Chem. Mater. 28, 3691–3702 (2016)

    CAS  Google Scholar 

  • Y. Sakamoto, S. Inagaki, T. Ohsuna, N. Ohnishi, Y. Fukushima, Y. Nozue, O. Terasaki: Structure analysis of mesoporous material ‘‘FSM-16'' studies by electron microscopy and x-ray diffraction, Microporous Mesoporous Mater. 21, 589–596 (1998)

    CAS  Google Scholar 

  • W.-X. Xu, J. Li, R.-P. Liu, W.-X. Zhou, W.-Y. Ma, F.-X. Zhang: A novel 1-D linear zinc(II) coordination polymer based 2,2′-bipyridine-4,4′-dicarboxylic acid: Synthesis, crystal structure and photoluminescence property, Inorg. Chem. Commun. 28, 12–15 (2013)

    CAS  Google Scholar 

  • A. Dhakshinamoorthy, M. Opanasenko, J. Čejka, H. Garcia: Metal organic frameworks as heterogeneous catalysts for the production of fine chemicals, Catal. Sci. Technol. 3, 2509–2540 (2013)

    CAS  Google Scholar 

  • J.A. Mason, M. Veenstra, J.R. Long: Evaluating metal-organic frameworks for natural gas storage, Chem. Sci. 5, 32–51 (2014)

    CAS  Google Scholar 

  • S.S. Kaye, A. Dailly, O.M. Yaghi, J.R. Long: Impact of preparation and handling on the hydrogen storage properties of Zn4O(1,4-benzenedicarboxylate)3 (MOF-5), J. Am. Chem. Soc. 129, 14176 (2007)

    CAS  Google Scholar 

  • S. Brunauer: Adsorption of gases in multimolecular layers, J. Am. Chem. Soc. 60, 309–319 (1938)

    CAS  Google Scholar 

  • J. Hafizovic, M. Bjørgen, U. Olsbye, P.D.C. Dietzel, S. Bordiga, C. Prestipino, C. Lamberti, K.P. Lillerud: The inconsistency in adsorption properties and powder XRD data of MOF-5 is rationalized by framework interpenetration and the presence of organic and inorganic species in the nanocavities, J. Am. Chem. Soc. 129, 3612–3620 (2007)

    CAS  Google Scholar 

  • M. Hmadeh, Z. Lu, Z. Liu, F. Gándara, H. Furukawa, S. Wan, V. Augustyn, R. Chang, L. Liao, F. Zhou, E. Perre, V. Ozolins, K. Suenaga, X. Duan, B. Dunn, Y. Yamamto, O. Terasaki, O.M. Yaghi: New porous crystals of extended metal-catecholates, Chem. Mater. 24, 3511–3513 (2012)

    CAS  Google Scholar 

  • A. Mayoral, M. Sanchez-Sanchez, A. Alfayate, J. Perez-Pariente, I. Díaz: Atomic observations of microporous materials highly unstable under the electron beam: The cases of Ti-doped AlPO4-5 and Zn-MOF-74, ChemCatChem 7, 3719–3724 (2015)

    CAS  Google Scholar 

  • M. Sánchez-Sánchez, N. Getachew, K. Díaz, M. Díaz-García, Y. Chebude, I. Díaz: Synthesis of metal-organic frameworks in water at room temperature: Salts as linker sources, Green Chem. 17, 1500–1509 (2015)

    Google Scholar 

  • A.T. Bell: The impact of nanoscience on heterogeneous catalysis, Science 299, 1688–1691 (2003)

    CAS  Google Scholar 

  • K. Egeblad, C.H. Christensen, M. Kustova, C.H. Christensen: Templating mesoporous zeolites, Chem. Mater. 20, 946–960 (2008)

    CAS  Google Scholar 

  • P. Horcajada, C. Serre, D. Grosso, C. Boissiere, S. Perruchas, C. Sanchez, G. Férey: Colloidal route for preparing optical thin films of nanoporous metal-organic frameworks, Adv. Mater. 21, 1931–1935 (2009)

    CAS  Google Scholar 

  • O. Shekhah, J. Liu, R.A. Fischer, C. Woell: MOF thin films: Existing and future applications, Chem. Soc. Rev. 40, 1081–1106 (2011)

    CAS  Google Scholar 

  • M. Ma, D. Zacher, X. Zhang, R.A. Fischer, N. Metzler-Nolte: A method for the preparation of highly porous, nanosized crystals of isoreticular metal-organic frameworks, Cryst. Growth Des. 11, 185–189 (2011)

    CAS  Google Scholar 

  • M. Díaz-García, Á. Mayoral, I. Díaz, M. Sánchez-Sánchez: Nanoscaled M-MOF-74 materials prepared at room temperature, Cryst. Growth Des. 14, 2479–2487 (2014)

    Google Scholar 

  • C. Serre, F. Millange, C. Thouvenot, M. Noguès, G. Marsolier, D. Louër, G. Férey: Very large breathing effect in the first nanoporous chromium(III)-based solids: MIL-53 or CrIII(OH)·{O2C−C6H4−CO2·{HO2C−C6H4−CO2Hx·H2Oy, J. Am. Chem. Soc. 124, 13519–13526 (2002)

    CAS  Google Scholar 

  • S. Bourrelly, P.L. Llewellyn, C. Serre, F. Millange, T. Loiseau, G. Férey: Different adsorption behaviors of methane and carbon dioxide in the isotypic nanoporous metal terephthalates MIL-53 and MIL-47, J. Am. Chem. Soc. 127, 13519–13521 (2005)

    CAS  Google Scholar 

  • P.L. Llewellyn, S. Bourrelly, C. Serre, Y. Filinchuk, G. Férey: How hydration drastically improves adsorption selectivity for CO2 over CH4 in the flexible chromium terephthalate MIL-53, Angew. Chem. Int. Ed. 45, 7751–7754 (2006)

    CAS  Google Scholar 

  • T. Loiseau, C. Serre, C. Huguenard, G. Fink, F. Taulelle, M. Henry, T. Bataille, G. Férey: A rationale for the large breathing of the porous aluminum terephthalate (MIL-53) upon hydration, Chem. Eur. J. 10, 1373–1382 (2004)

    CAS  Google Scholar 

  • Y. Liu, J.H. Her, A. Dailly, A.J. Ramirez-Cuesta, D.A. Neumann, C.M. Brown: Reversible structural transition in MIL-53 with large temperature hysteresis, J. Am. Chem. Soc. 130, 11813–11818 (2008)

    CAS  Google Scholar 

  • F. Millange, C. Serre, G. Férey: Synthesis, structure determination and properties of MIL-53as and MIL-53ht: The first CrIII hybrid inorganic-organic microporous solids: CrIII(OH)·{O2C–C6H4–CO2·{HO2C–C6H4–CO2Hx, Chem. Commun. (2002), https://doi.org/10.1039/B201381A

    Article  Google Scholar 

  • B. Seoane, S. Sorribas, A. Mayoral, C. Tellez, J. Coronas: Real-time monitoring of breathing of MIL-53(Al) by environmental SEM, Microporous Mesoporous Mater. 203, 17–23 (2015)

    CAS  Google Scholar 

  • M. Maes, F. Vermoortele, L. Alaerts, S. Couck, C.E.A. Kirschhock, J.F.M. Denayer, D.E. De Vos: Separation of styrene and ethylbenzene on metal-organic frameworks: Analogous structures with different adsorption mechanisms, J. Am. Chem. Soc. 132, 15277–15285 (2010)

    CAS  Google Scholar 

  • V. Finsy, C.E.A. Kirschhock, G. Vedts, M. Maes, L. Alaerts, D.E. De Vos, G.V. Baron, J.F.M. Denayer: Framework breathing in the vapour-phase adsorption and separation of xylene isomers with the metal-organic framework MIL-53, Chem. Eur. J. 15, 7724–7731 (2009)

    CAS  Google Scholar 

  • Y. Zhu, J. Ciston, B. Zheng, X. Miao, C. Czarnik, Y. Pan, R. Sougrat, Z. Lai, C.-E. Hsiung, K. Yao, I. Pinnau, M. Pan, Y. Han: Unravelling surface and interfacial structures of a metal-organic framework by transmission electron microscopy, Nat. Mater. 16, 532–536 (2017)

    CAS  Google Scholar 

  • D. Zhang, Y. Zhu, L. Liu, X. Ying, C.-E. Hsiung, R. Sougrat, K. Li, Y. Han: Atomic-resolution transmission electron microscopy of electron beam–sensitive crystalline materials, Science 359(6376), 675–679 (2018)

    CAS  Google Scholar 

  • K. Shen, L. Zhang, X. Chen, L. Liu, D. Zhang, Y. Han, J. Chen, J. Long, R. Luque, Y. Li, B. Chen: Ordered macro-microporous metal-organic framework single crystals, Science 359, 206–210 (2018)

    CAS  Google Scholar 

  • T.J. Woehl, K.L. Jungjohann, J.E. Evans, I. Arslan, W.D. Ristenpart, N.D. Browning: Experimental procedures to mitigate electron beam induced artifacts during in situ fluid imaging of nanomaterials, Ultramicroscopy 127, 53–63 (2013)

    CAS  Google Scholar 

  • J.P. Patterson, P. Abellan, M.S.J. Denny, C. Park, N.D. Browning, S.M. Cohen, J.F. Evans, N.C. Gianneschi: Observing the growth of metal-organic frameworks by in situ liquid cell transmission electron microscopy, J. Am. Chem. Soc. 137, 7322–7328 (2015)

    CAS  Google Scholar 

  • S.R. Venna, J.B. Jasinski, M.A. Carreon: Structural evolution of zeolitic imidazolate framework-8, J. Am. Chem. Soc. 132, 18030–18033 (2010)

    CAS  Google Scholar 

  • K. Guesh, C.A.D. Caiuby, Á. Mayoral, M. Díaz-García, I. Díaz, M. Sanchez-Sanchez: Sustainable preparation of MIL-100(Fe) and its photocatalytic behavior in the degradation of methyl orange in water, Cryst. Growth Des. 17, 1806–1813 (2017)

    CAS  Google Scholar 

  • M. Sanchez-Sanchez, I. de Asua, D. Ruano, K. Diaz: Direct synthesis, structural features, and enhanced catalytic activity of the basolite F300-like semiamorphous Fe-BTC framework, Cryst. Growth Des. 15, 4498–4506 (2015)

    CAS  Google Scholar 

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Acknowledgements

This work was supported by the Shanghai Pujiang Program (17PJ1406400), Shanghai Natural Science Fund (17ZR1418600), the Young Elite Scientist Sponsorship Program By CAST (2017QNRC001) (Y.M.), the National Natural Science Foundation of China 21571128, the National Excellent Doctoral Dissertation of China 201454, and the Shanghai Rising Star Program 17QA1401700 (L.H.), JST (Japan), VR and Wallenberg Foundation (Sweden) and Foreign Expert Recruiting Program (China) (O.T.). This work is partially supported by CℏEM, SPST, ShanghaiTech under the grant #EM02161943 (Y.M., A.M., P.O. and O.T.). O.T. acknowledges Sir John Meurig Thomas for introducing and guiding him to his fascinating field, the structural study of nanostructured materials by electron crystallography and imaging.

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Correspondence to Osamu Terasaki .

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Ma, Y. et al. (2019). Microscopy of Nanoporous Crystals. In: Hawkes, P.W., Spence, J.C.H. (eds) Springer Handbook of Microscopy. Springer Handbooks. Springer, Cham. https://doi.org/10.1007/978-3-030-00069-1_29

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