Endre søk
RefereraExporteraLink to record
Permanent link

Direct link
Referera
Referensformat
  • apa
  • ieee
  • modern-language-association-8th-edition
  • vancouver
  • Annet format
Fler format
Språk
  • de-DE
  • en-GB
  • en-US
  • fi-FI
  • nn-NO
  • nn-NB
  • sv-SE
  • Annet språk
Fler språk
Utmatningsformat
  • 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
Stockholms universitet, Naturvetenskapliga fakulteten, Institutionen för material- och miljökemi (MMK).
Stockholms universitet, Naturvetenskapliga fakulteten, Institutionen för material- och miljökemi (MMK).
Stockholms universitet, Naturvetenskapliga fakulteten, Institutionen för material- och miljökemi (MMK).
Stockholms universitet, Naturvetenskapliga fakulteten, Institutionen för material- och miljökemi (MMK).
Vise andre og tillknytning
2014 (engelsk)Inngår i: Crystal Growth & Design, ISSN 1528-7483, E-ISSN 1528-7505, Vol. 14, nr 10, s. 5072-5078Artikkel i tidsskrift (Fagfellevurdert) 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.

sted, utgiver, år, opplag, sider
2014. Vol. 14, nr 10, s. 5072-5078
HSV kategori
Identifikatorer
URN: urn:nbn:se:su:diva-102757DOI: 10.1021/cg500681kISI: 000342609300027OAI: oai:DiVA.org:su-102757DiVA, id: diva2:713237
Tilgjengelig fra: 2014-04-22 Laget: 2014-04-22 Sist oppdatert: 2017-12-05bibliografisk kontrollert
Inngår i avhandling
1. Inorganic and Metal-Organic Framework Materials: Synthesis and structure characterization
Åpne denne publikasjonen i ny fane eller vindu >>Inorganic and Metal-Organic Framework Materials: Synthesis and structure characterization
2014 (engelsk)Doktoravhandling, med artikler (Annet vitenskapelig)
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.

sted, utgiver, år, opplag, sider
Department of Materials and Environmental Chemistry (MMK), Stockholm University, 2014. s. 86
Emneord
X-ray diffraction, transmission electron microscopy, framework materials, porous materials
HSV kategori
Forskningsprogram
oorganisk kemi
Identifikatorer
urn:nbn:se:su:diva-102816 (URN)978-91-7447-913-3 (ISBN)
Disputas
2014-05-28, Magnélisalen, Kemiska övningslaboratoriet, Svante Arrhenius väg 16 B, Stockholm, 10:00 (engelsk)
Opponent
Veileder
Merknad

At the time of the doctoral defence the following paper was unpublished and a status as follows: Paper  4: Manuscript

Tilgjengelig fra: 2014-05-06 Laget: 2014-04-22 Sist oppdatert: 2014-05-02bibliografisk kontrollert
2. Characterization of crystalline materials by rotation electron diffraction: Phase identification and structure determination
Åpne denne publikasjonen i ny fane eller vindu >>Characterization of crystalline materials by rotation electron diffraction: Phase identification and structure determination
2014 (engelsk)Doktoravhandling, med artikler (Annet vitenskapelig)
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.

sted, utgiver, år, opplag, sider
Stockholm: Department of Materials and Environmental Chemistry (MMK), Stockholm University, 2014. s. 102
Emneord
electron microscopy, phase identification, rotation electron diffraction, structure determination, three-dimensional electron diffraction
HSV kategori
Forskningsprogram
oorganisk kemi
Identifikatorer
urn:nbn:se:su:diva-108930 (URN)978-91-7649-017-4 (ISBN)
Disputas
2014-12-17, Magnélisalen, Kemiska övningslaboratoriet, Svante Arrhenius väg 16 B, Stockholm, 10:00 (engelsk)
Opponent
Veileder
Merknad

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.

Tilgjengelig fra: 2014-11-25 Laget: 2014-11-06 Sist oppdatert: 2015-10-27bibliografisk kontrollert

Open Access i DiVA

Fulltekst mangler i DiVA

Andre lenker

Forlagets fulltekst

Søk i DiVA

Av forfatter/redaktør
Fang, LiangLiu, LeifengYun, YifengWan, WeiZou, Xiaodong
Av organisasjonen
I samme tidsskrift
Crystal Growth & Design

Søk utenfor DiVA

GoogleGoogle Scholar

doi
urn-nbn

Altmetric

doi
urn-nbn
Totalt: 134 treff
RefereraExporteraLink to record
Permanent link

Direct link
Referera
Referensformat
  • apa
  • ieee
  • modern-language-association-8th-edition
  • vancouver
  • Annet format
Fler format
Språk
  • de-DE
  • en-GB
  • en-US
  • fi-FI
  • nn-NO
  • nn-NB
  • sv-SE
  • Annet språk
Fler språk
Utmatningsformat
  • html
  • text
  • asciidoc
  • rtf