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Inorganic and Metal-Organic Framework Materials: Synthesis and structure characterization
Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK).
2014 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

Inorganic and metal-organic framework materials possessing accessible and permanent pores are receiving tremendous attention. Among them, zeolites are the most famous class due to their wide applications on petrochemistry and gas separation. Besides zeolites, the other oxide framework materials are also intensively investigated because of their diverse structures and compositions. Metal-organic frameworks are built from metal clusters and organic linkers. By rational designing the reagent, the network with desired topology and functionality can be synthesized.

For all of the framework materials mentioned above, to explore novel framework structures is important for improving properties and discovering new applications. This thesis includes the synthesis of zeolites and structure characterization for various types of inorganic framework materials. The zeolite synthesis conditions was exploited. With the optimized condition, the zeolite ITQ-33 was synthesized as single crystals. From the single crystal X-ray diffraction data, the disorder in the structure is discovered and explained. Following the topic of disorder and twinning, we proposed a novel method of solving structure of pseudo-merohedric twinning crystal by using an example of a metal-organic complex crystal. Then we also showed methods for solving structures of high complexity and nano-crystal by using mainly powder X-ray diffraction and transmission electron microscopy. Four examples were shown in chapter 4 including open-framework germanates and metal-organic frameworks.

Place, publisher, year, edition, pages
Department of Materials and Environmental Chemistry (MMK), Stockholm University , 2014. , 86 p.
Keyword [en]
X-ray diffraction, transmission electron microscopy, framework materials, porous materials
National Category
Inorganic Chemistry
Research subject
Inorganic Chemistry
Identifiers
URN: urn:nbn:se:su:diva-102816ISBN: 978-91-7447-913-3 (print)OAI: oai:DiVA.org:su-102816DiVA: diva2:713389
Public defence
2014-05-28, Magnélisalen, Kemiska övningslaboratoriet, Svante Arrhenius väg 16 B, Stockholm, 10:00 (English)
Opponent
Supervisors
Note

At the time of the doctoral defence the following paper was unpublished and a status as follows: Paper  4: Manuscript

Available from: 2014-05-06 Created: 2014-04-22 Last updated: 2014-05-02Bibliographically approved
List of papers
1. Disorder in Extra-Large Pore Zeolite ITQ-33 Revealed by Single Crystal XRD
Open this publication in new window or tab >>Disorder in Extra-Large Pore Zeolite ITQ-33 Revealed by Single Crystal XRD
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2013 (English)In: Crystal Growth & Design, ISSN 1528-7483, E-ISSN 1528-7505, Vol. 13, no 10, 4168-4171 p.Article in journal (Refereed) Published
Abstract [en]

The single crystal of the extra-large pore zeolite, ITQ-33, was obtained and used to explore its crystal structure details. The ITQ-33 structure was found to be disordered with the columnar periodic building unit, explaining the morphology changes upon the different Si/Ge ratio, and the formation of the hierarchical structure from assembling of ITQ-33 nanofibers.

National Category
Organic Chemistry Inorganic Chemistry
Identifiers
urn:nbn:se:su:diva-97039 (URN)10.1021/cg400880a (DOI)000326300200005 ()
Funder
Swedish Research CouncilVinnovaKnut and Alice Wallenberg Foundation
Note

AuthorCount:6;

Available from: 2013-12-03 Created: 2013-12-02 Last updated: 2017-12-06Bibliographically approved
2. Structure determination of [3Fe2S] complex with complicated pseudo-merohedric twinning
Open this publication in new window or tab >>Structure determination of [3Fe2S] complex with complicated pseudo-merohedric twinning
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2012 (English)In: Zeitschrift fur Kristallographie, ISSN 0044-2968, Vol. 227, no 4, 221-226 p.Article in journal (Refereed) Published
Abstract [en]

A route of solving crystal structures from complicated pseudo-merohedric twinning crystals was described. The structure of a [3Fe2S] complex was solved and refined in the space group of P42/n to R1 factor of 0.1789. Consequently, by deleting one of the two disordered groups in the structure, a space group of Aea2 for the absolute structure was found. The new absolute structure with four twinning components was refined to R1 about 0.1171. At the final stage, the disorder was again added to the structure. The structure in space group Aea2 with both twinning and disorder was refined to R1 of 0.0722, which implies the special structure feature.

Keyword
Space group determination, Disorder, Twinning, Single crystal structure analysis, X-ray diffraction
National Category
Chemical Sciences
Identifiers
urn:nbn:se:su:diva-79712 (URN)10.1524/zkri.2012.1502 (DOI)000303283300005 ()
Funder
Swedish Research CouncilKnut and Alice Wallenberg Foundation
Note

AuthorCount:5;

Available from: 2012-09-14 Created: 2012-09-11 Last updated: 2017-12-07Bibliographically approved
3. Germanate with Three-Dimensional 12 x 12 x 11-Ring Channels Solved by X-ray Powder Diffraction with Charge-Flipping Algorithm
Open this publication in new window or tab >>Germanate with Three-Dimensional 12 x 12 x 11-Ring Channels Solved by X-ray Powder Diffraction with Charge-Flipping Algorithm
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2013 (English)In: Inorganic Chemistry, ISSN 0020-1669, E-ISSN 1520-510X, Vol. 52, no 18, 10238-10244 p.Article in journal (Refereed) Published
Abstract [en]

A new open-framework germanate, denoted as GeO-JU90, was prepared by the hydrothermal synthesis method using 1,5-bis(methylpyrrolidinium)pentane dihydroxide as the organic structure-directing agent (SDA). The structure of GeO-JU90 was determined from synchrotron X-ray powder diffraction (XRPD) data using the charge-flipping algorithm. It revealed a complicated framework structure containing 11 Ge atoms in the asymmetric unit. The framework is built of 7-connected Ge-7 clusters and additional tetrahedral GeO3(OH) units forming a new three-dimensional interrupted framework with interesting 12 X 12 X 11-ring intersecting channels. The Ge K-edge extended X-ray absorption fine structure (EXAFS) analysis was performed to provide the local structural information around Ge atoms, giving rise to a first-shell contribution from about 4.2(2) O atoms at the average distance of 1.750(8) angstrom. The guest species subsequently determined by the simulated annealing method from XRPD data combining with other characterization techniques, e.g., C-13 NMR spectroscopy, infrared spectroscopy (FTIR), compositional analyses, and thermogravimetric analysis (TGA). Crystallographic data vertical bar(C15N2H32)(NH4)vertical bar[Ge11O21.5(OH)(4)], orthorhombic Ama2 (No. 40), a = 37.82959 angstrom, b = 15.24373 angstrom, c = 12.83659 angstrom, and Z = 8.

National Category
Chemical Sciences
Identifiers
urn:nbn:se:su:diva-101026 (URN)10.1021/ic302705f (DOI)000330098300008 ()
Note

AuthorCount:6;

Funding agencies:

National Natural Science Foundation of China;  State Basic Research Project of China 2011CB808703; Swedish Research Council (VR);  Swedish Governmental Agency for Innovation Systems (VINNOVA) through the Berzelii Center EXSELENT;  NSERC Canada;  CIHR;  NRC; University of Saskatchewan  

Available from: 2014-02-27 Created: 2014-02-21 Last updated: 2017-12-05Bibliographically approved
4. SU-77: An Open-Framework Germanate Containing 12 × 10 × 10-Ring Channels Solved by Combining Rotation Electron Diffraction and Powder X-ray Diffraction
Open this publication in new window or tab >>SU-77: An Open-Framework Germanate Containing 12 × 10 × 10-Ring Channels Solved by Combining Rotation Electron Diffraction and Powder X-ray Diffraction
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2014 (English)In: Crystal Growth & Design, ISSN 1528-7483, E-ISSN 1528-7505, Vol. 14, no 10, 5072-5078 p.Article in journal (Refereed) Published
Abstract [en]

A novel open-framework germanate, denoted as SU-77, was prepared by hydrothermal synthesis using ethylenediamine as the structure directing agent. The as-synthesized SU-77 is monoclinic with space group P21/a and a = 13.52427(5) Å, b = 12.64862(5) Å, c = 9.60578(3) Å, β = 92.8599(4)°. The structure of SU-77 is built from a novel Ge6O17(C2H8N2)F (Ge6) cluster building unit. The Ge6 clusters are connected to form chains along the c-axis. These chains are further connected in the [110] and [1–10] directions to form a three-dimensional framework with 12 × 10 × 10-ring channels. The as-synthesized monoclinic SU-77 became orthorhombic while being observed in a transmission electron microscope (TEM) or when heated to 200 °C in air. The orthorhombic structure of SU-77 was solved from micrometer-sized crystals by rotation electron diffraction (RED). The monoclinic structure was built from the orthorhombic structure and subsequently refined against synchrotron powder X-ray diffraction data. SU-77 is the first example of an open-framework germanate with mixed coordination polyhedra solved by electron diffraction.

National Category
Inorganic Chemistry
Identifiers
urn:nbn:se:su:diva-102757 (URN)10.1021/cg500681k (DOI)000342609300027 ()
Available from: 2014-04-22 Created: 2014-04-22 Last updated: 2017-12-05Bibliographically approved
5. Metal-Oxide Nanoparticles with Desired Morphology Inherited from Coordination-Polymer Precursors
Open this publication in new window or tab >>Metal-Oxide Nanoparticles with Desired Morphology Inherited from Coordination-Polymer Precursors
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2012 (English)In: Chemistry - A European Journal, ISSN 0947-6539, E-ISSN 1521-3765, Vol. 18, no 11, 3163-3168 p.Article in journal (Refereed) Published
Abstract [en]

The “escape-by-crafty-scheme” strategy is an efficient approach to prepare metal-oxide nanomaterials with desirable morphology and crystal planes inherited from coordination-polymer nanoparticle precursors, which can be designed and finely tuned by soft chemical assembly of metal ions and organic ligands at the molecular level (see scheme; ptcda=perylene-3,4,9,10-tetracarboxylic dianhydride).

Keyword
hydrothermal synthesis, metal oxides, metal-organic frameworks, morphologies, nanoparticles
National Category
Chemical Sciences
Identifiers
urn:nbn:se:su:diva-76278 (URN)10.1002/chem.201103415 (DOI)000300972500011 ()
Note
7Available from: 2012-05-16 Created: 2012-05-10 Last updated: 2017-12-07Bibliographically approved
6. Irreversible Network Transformation in a Dynamic Porous Host Catalyzed by Sulfur Dioxide
Open this publication in new window or tab >>Irreversible Network Transformation in a Dynamic Porous Host Catalyzed by Sulfur Dioxide
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2013 (English)In: Journal of the American Chemical Society, ISSN 0002-7863, E-ISSN 1520-5126, Vol. 135, no 13, 4954-4957 p.Article in journal (Refereed) Published
Abstract [en]

Porous NOTT-202a shows exceptionally high uptake of SO2, 13.6 mmol g(-1) (87.0 wt %) at 268 K and 1.0 bar, representing the highest value reported to date for a framework material. NOTT-202a undergoes a distinct irreversible framework phase transition upon SO2 uptake at 268-283 K to give NOTT-202b which has enhanced stability due to the formation of strong pi...pi interactions between interpenetrated networks.

National Category
Chemical Sciences
Identifiers
urn:nbn:se:su:diva-89994 (URN)10.1021/ja401061m (DOI)000317259300014 ()
Funder
Swedish Research Council
Note

AuthorCount:11;

Available from: 2013-05-20 Created: 2013-05-20 Last updated: 2017-12-06Bibliographically approved

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