Details
| Original language | English |
|---|---|
| Pages (from-to) | 141-159 |
| Number of pages | 19 |
| Journal | Zeitschrift fur Kristallographie - Crystalline Materials |
| Volume | 232 |
| Issue number | 1-3 |
| Publication status | Published - 1 Feb 2017 |
Abstract
In this contribution we report on the development and application of modern NMR approaches for the in situ characterization of the crystallization of metastable materials. The work was performed within the framework of the DFG priority programme SPP 1415 "Crystalline Non- Equilibrium Phases". As one of the goals of this project, the development of a NMR methodology which enables an analysis of local structural motifs on short (1-2 A) and extended (2-6 A) length scales without the need for fast magic angle spinning (MAS) has been defined, since the enormous centripetal forces which occur during fast sample rotation (up to 107 g) may intervene with the chemical or physical process which is being monitored. To achieve this goal, we developed a magic angle turning probe and pulse sequences allowing to trace the isotropic chemical shifts and heteronuclear dipolar couplings and hence the determination of structural motifs on short and intermediate length scales. With the implementation of novel inductive heating approaches the range of accessible rotation frequencies for in situ high temperature NMR measurements has been enlarged, now covering the ?MAS range of 0-10 kHz with an accessible temperature of up to 700 °C. Application of NMR methodologies for the characterization of crystallization processes and the structure and dynamics of novel phases, partially in joint collaborations within the priority program, are also reported.
Keywords
- Crystallization processes, Ionic conductors, Solid state NMR
ASJC Scopus subject areas
- Materials Science(all)
- General Materials Science
- Physics and Astronomy(all)
- Condensed Matter Physics
- Chemistry(all)
- Inorganic Chemistry
Cite this
- Standard
- Harvard
- Apa
- Vancouver
- BibTeX
- RIS
In: Zeitschrift fur Kristallographie - Crystalline Materials, Vol. 232, No. 1-3, 01.02.2017, p. 141-159.
Research output: Contribution to journal › Article › Research › peer review
}
TY - JOUR
T1 - Development and application of novel NMR methodologies for the in situ characterization of crystallization processes of metastable crystalline materials
AU - Van Wüllen, Leo
AU - Schiffmann, Jan Gerrit
AU - Kopp, Jakob
AU - Liu, Zhongqing
AU - Kirchhain, Holger
AU - Düvel, André
AU - Heitjans, Paul
N1 - Funding Information: We gratefully acknowledge funding by the Deutsche Forschungsgemeinschaft within the priority programme SPP 1415. Collaborations and fruitful discussions within numerous members of the priority programme, especially with T. Nilges and M. Wiebcke are also cordially acknowledged. Copyright: Copyright 2017 Elsevier B.V., All rights reserved.
PY - 2017/2/1
Y1 - 2017/2/1
N2 - In this contribution we report on the development and application of modern NMR approaches for the in situ characterization of the crystallization of metastable materials. The work was performed within the framework of the DFG priority programme SPP 1415 "Crystalline Non- Equilibrium Phases". As one of the goals of this project, the development of a NMR methodology which enables an analysis of local structural motifs on short (1-2 A) and extended (2-6 A) length scales without the need for fast magic angle spinning (MAS) has been defined, since the enormous centripetal forces which occur during fast sample rotation (up to 107 g) may intervene with the chemical or physical process which is being monitored. To achieve this goal, we developed a magic angle turning probe and pulse sequences allowing to trace the isotropic chemical shifts and heteronuclear dipolar couplings and hence the determination of structural motifs on short and intermediate length scales. With the implementation of novel inductive heating approaches the range of accessible rotation frequencies for in situ high temperature NMR measurements has been enlarged, now covering the ?MAS range of 0-10 kHz with an accessible temperature of up to 700 °C. Application of NMR methodologies for the characterization of crystallization processes and the structure and dynamics of novel phases, partially in joint collaborations within the priority program, are also reported.
AB - In this contribution we report on the development and application of modern NMR approaches for the in situ characterization of the crystallization of metastable materials. The work was performed within the framework of the DFG priority programme SPP 1415 "Crystalline Non- Equilibrium Phases". As one of the goals of this project, the development of a NMR methodology which enables an analysis of local structural motifs on short (1-2 A) and extended (2-6 A) length scales without the need for fast magic angle spinning (MAS) has been defined, since the enormous centripetal forces which occur during fast sample rotation (up to 107 g) may intervene with the chemical or physical process which is being monitored. To achieve this goal, we developed a magic angle turning probe and pulse sequences allowing to trace the isotropic chemical shifts and heteronuclear dipolar couplings and hence the determination of structural motifs on short and intermediate length scales. With the implementation of novel inductive heating approaches the range of accessible rotation frequencies for in situ high temperature NMR measurements has been enlarged, now covering the ?MAS range of 0-10 kHz with an accessible temperature of up to 700 °C. Application of NMR methodologies for the characterization of crystallization processes and the structure and dynamics of novel phases, partially in joint collaborations within the priority program, are also reported.
KW - Crystallization processes
KW - Ionic conductors
KW - Solid state NMR
UR - http://www.scopus.com/inward/record.url?scp=85011923701&partnerID=8YFLogxK
U2 - 10.1515/zkri-2016-1975
DO - 10.1515/zkri-2016-1975
M3 - Article
AN - SCOPUS:85011923701
VL - 232
SP - 141
EP - 159
JO - Zeitschrift fur Kristallographie - Crystalline Materials
JF - Zeitschrift fur Kristallographie - Crystalline Materials
SN - 2194-4946
IS - 1-3
ER -