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Development and application of novel NMR methodologies for the in situ characterization of crystallization processes of metastable crystalline materials

  • Leo van Wüllen EMAIL logo , Jan Gerrit Schiffmann , Jakob Kopp , Zhongqing Liu , Holger Kirchhain , Andre Düvel and Paul Heitjans EMAIL logo
Published/Copyright: November 8, 2016
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Zeitschrift für Kristallographie - Crystalline Materials
From the journal Zeitschrift für Kristallographie - Crystalline Materials Volume 232 Issue 1-3

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 Å) and extended (2–6 Å) 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 νMAS 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

Acknowledgments

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.

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Received: 2016-6-10
Accepted: 2016-9-6
Published Online: 2016-11-8
Published in Print: 2017-2-1

©2017 Walter de Gruyter GmbH, Berlin/Boston

Articles in the same Issue

  1. Frontmatter
  2. Graphical Synopsis
  3. Editorial
  4. Synthesis and characterization of metastable transition metal oxides and oxide nitrides
  5. Control of organic polymorph formation: crystallization pathways in acoustically levitated droplets
  6. Thermal annealing of natural, radiation-damaged pyrochlore
  7. The formation of CdS quantum dots and Au nanoparticles
  8. Crystalline chalcogenido metalates – synthetic approaches for materials synthesis and transformation
  9. Fundamental theoretical and practical investigations of the polymorph formation of small amphiphilic molecules, their co-crystals and salts
  10. A density-functional theory approach to the existence and stability of molybdenum and tungsten sesquioxide polymorphs
  11. The ZIF system zinc(II) 4,5-dichoroimidazolate: theoretical and experimental investigations of the polymorphism and crystallization mechanisms
  12. Element allotropes and polyanion compounds of pnicogenes and chalcogenes: stability, mechanisms of formation, controlled synthesis and characterization
  13. Structure and ion dynamics of mechanosynthesized oxides and fluorides
  14. Scaled-up solvothermal synthesis of nanosized metastable indium oxyhydroxide (InOOH) and corundum-type rhombohedral indium oxide (rh-In2O3)
  15. Development and application of novel NMR methodologies for the in situ characterization of crystallization processes of metastable crystalline materials
  16. Phase formation and stability in TiOx and ZrOx thin films: Extremely sub-stoichiometric functional oxides for electrical and TCO applications
  17. Investigations on the growth of bismuth oxido clusters and the nucleation to give metastable bismuth oxide modifications
  18. Divalent metal phosphonates – new aspects for syntheses, in situ characterization and structure solution
  19. Type-I silicon clathrates containing lithium
  20. Experimental and theoretical investigation of the chromium–vanadium–antimony system
  21. Synthesis and crystal structure of three new bismuth(III) arylsulfonatocarboxylates
  22. Snapshots of calcium carbonate formation – a step by step analysis
https://doi.org/10.1515/zkri-2016-1975
Keywords for this article
crystallization processes; ionic conductors; solid state NMR

Articles in the same Issue

  1. Frontmatter
  2. Graphical Synopsis
  3. Editorial
  4. Synthesis and characterization of metastable transition metal oxides and oxide nitrides
  5. Control of organic polymorph formation: crystallization pathways in acoustically levitated droplets
  6. Thermal annealing of natural, radiation-damaged pyrochlore
  7. The formation of CdS quantum dots and Au nanoparticles
  8. Crystalline chalcogenido metalates – synthetic approaches for materials synthesis and transformation
  9. Fundamental theoretical and practical investigations of the polymorph formation of small amphiphilic molecules, their co-crystals and salts
  10. A density-functional theory approach to the existence and stability of molybdenum and tungsten sesquioxide polymorphs
  11. The ZIF system zinc(II) 4,5-dichoroimidazolate: theoretical and experimental investigations of the polymorphism and crystallization mechanisms
  12. Element allotropes and polyanion compounds of pnicogenes and chalcogenes: stability, mechanisms of formation, controlled synthesis and characterization
  13. Structure and ion dynamics of mechanosynthesized oxides and fluorides
  14. Scaled-up solvothermal synthesis of nanosized metastable indium oxyhydroxide (InOOH) and corundum-type rhombohedral indium oxide (rh-In2O3)
  15. Development and application of novel NMR methodologies for the in situ characterization of crystallization processes of metastable crystalline materials
  16. Phase formation and stability in TiOx and ZrOx thin films: Extremely sub-stoichiometric functional oxides for electrical and TCO applications
  17. Investigations on the growth of bismuth oxido clusters and the nucleation to give metastable bismuth oxide modifications
  18. Divalent metal phosphonates – new aspects for syntheses, in situ characterization and structure solution
  19. Type-I silicon clathrates containing lithium
  20. Experimental and theoretical investigation of the chromium–vanadium–antimony system
  21. Synthesis and crystal structure of three new bismuth(III) arylsulfonatocarboxylates
  22. Snapshots of calcium carbonate formation – a step by step analysis
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