Change search
CiteExportLink to record
Permanent link

Direct link
Cite
Citation style
  • apa
  • ieee
  • modern-language-association-8th-edition
  • vancouver
  • Other style
More styles
Language
  • de-DE
  • en-GB
  • en-US
  • fi-FI
  • nn-NO
  • nn-NB
  • sv-SE
  • Other locale
More languages
Output format
  • html
  • text
  • asciidoc
  • rtf
SU-77: An Open-Framework Germanate Containing 12 × 10 × 10-Ring Channels Solved by Combining Rotation Electron Diffraction and Powder X-ray Diffraction
Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK).
Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK).
Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK).
Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK).
Show others and affiliations
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.

Place, publisher, year, edition, pages
2014. Vol. 14, no 10, 5072-5078 p.
National Category
Inorganic Chemistry
Identifiers
URN: urn:nbn:se:su:diva-102757DOI: 10.1021/cg500681kISI: 000342609300027OAI: oai:DiVA.org:su-102757DiVA: diva2:713237
Available from: 2014-04-22 Created: 2014-04-22 Last updated: 2017-12-05Bibliographically approved
In thesis
1. Inorganic and Metal-Organic Framework Materials: Synthesis and structure characterization
Open this publication in new window or tab >>Inorganic and Metal-Organic Framework Materials: Synthesis and structure characterization
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
X-ray diffraction, transmission electron microscopy, framework materials, porous materials
National Category
Inorganic Chemistry
Research subject
Inorganic Chemistry
Identifiers
urn:nbn:se:su:diva-102816 (URN)978-91-7447-913-3 (ISBN)
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
2. Characterization of crystalline materials by rotation electron diffraction: Phase identification and structure determination
Open this publication in new window or tab >>Characterization of crystalline materials by rotation electron diffraction: Phase identification and structure determination
2014 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

Electron crystallography is powerful for determination of complex structures. The newly-developed 3D electron diffraction (ED) methods make structure determination from nano- and micron-sized crystals much easier than using other methods, for example X-ray diffraction. Almost complete 3D ED data can be collected easily and fast from crystals at any arbitrary orientations. Dynamical effects are largely reduced compared to zonal ED patterns. 3D ED is powerful for phase identification and structure solution from individual nano- and micron-sized crystals, while powder X-ray diffraction (PXRD) provides information from all phases present in the samples. 3D ED methods and PXRD are complementary and their combinations are promising for studying multiphasic samples and complicated crystal structures.

In this thesis, the feasibility and capability of 3D ED methods, specifically rotation electron diffraction (RED), in phase identification and structure determination of different kinds of crystalline materials with nano- or submicrometer-sized crystals are investigated. Experimental conditions for RED data collection and data processing in relation to data quality, as well as the challenges in the applications of RED are discussed.

RED was combined with PXRD to identify phases from as-synthesized samples and to characterize atomic structures of eleven crystalline compounds. It was shown to be possible to identify as many as four distinct compounds within one sample containing submicron-sized crystals in a Ni-Se-O-Cl system. RED was also used to determine unit cell and symmetry of isoreticular metal-organic frameworks (SUMOF-7) and solve five zeolite structures with new frameworks, ITQ-51, ITQ-53, ITQ-54, EMM-23 and EMM-25 and that of a metal-organic framework (MOF), SUMOF-7I. The structure of an open-framework germanate SU-77 was solved by combining RED with PXRD. The structures of the zeolites and SU-77 were confirmed by Rietveld refinement against PXRD. High-resolution transmission electron microscopy was used to confirm the structure models of ITQ-51, EMM-25 and SUMOF-7I.

Place, publisher, year, edition, pages
Stockholm: Department of Materials and Environmental Chemistry (MMK), Stockholm University, 2014. 102 p.
Keyword
electron microscopy, phase identification, rotation electron diffraction, structure determination, three-dimensional electron diffraction
National Category
Inorganic Chemistry
Research subject
Inorganic Chemistry
Identifiers
urn:nbn:se:su:diva-108930 (URN)978-91-7649-017-4 (ISBN)
Public defence
2014-12-17, Magnélisalen, Kemiska övningslaboratoriet, Svante Arrhenius väg 16 B, Stockholm, 10:00 (English)
Opponent
Supervisors
Note

At the time of the doctoral defense, the following papers were unpublished and had a status as follows: Paper 2: Submitted. Paper 4: Accepted. Paper 6: Manuscript. Paper 7: Epub ahead of print. Paper 9: Manuscript. Paper 11: Manuscript.

Available from: 2014-11-25 Created: 2014-11-06 Last updated: 2015-10-27Bibliographically approved

Open Access in DiVA

No full text

Other links

Publisher's full text

Search in DiVA

By author/editor
Fang, LiangLiu, LeifengYun, YifengWan, WeiZou, Xiaodong
By organisation
Department of Materials and Environmental Chemistry (MMK)
In the same journal
Crystal Growth & Design
Inorganic Chemistry

Search outside of DiVA

GoogleGoogle Scholar

doi
urn-nbn

Altmetric score

doi
urn-nbn
Total: 122 hits
CiteExportLink to record
Permanent link

Direct link
Cite
Citation style
  • apa
  • ieee
  • modern-language-association-8th-edition
  • vancouver
  • Other style
More styles
Language
  • de-DE
  • en-GB
  • en-US
  • fi-FI
  • nn-NO
  • nn-NB
  • sv-SE
  • Other locale
More languages
Output format
  • html
  • text
  • asciidoc
  • rtf