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Updated: Jan 4, 2026
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Methods of Ex Situ and In Situ Investigations of Structural Transformations: The Case of Crystallization of Metallic Glasses
Published on: June 7, 2018
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In situ solid-state NMR of a magnetically oriented microcrystal suspension
Ryosuke Kusumi1, Hiroshi Kadoma1, Masahisa Wada2
1Division of Forest and Biomaterials Science, Graduate School of Agriculture, Kyoto University, Kyoto 606-8502, Japan.
Journal of Magnetic Resonance (San Diego, Calif. : 1997)
|November 1, 2019
Summary
This study introduces a novel 3D-MOMS technique for solid-state NMR. It enables magnetic alignment of microcrystals, simplifying single-crystal rotation patterns without complex adjustments.
Area of Science:
- Solid-state Nuclear Magnetic Resonance (NMR) spectroscopy.
- Materials science and crystallography.
Background:
- Traditional single-crystal (SC) NMR methods require complex sample manipulation and alignment.
- Microcrystalline samples often present challenges for detailed structural analysis using NMR.
Purpose of the Study:
- To develop a new method for obtaining SC NMR data from microcrystalline samples.
- To demonstrate the utility of magnetically oriented microcrystal suspension (MOMS) for 3D structural analysis.
Main Methods:
- Utilized in situ solid-state NMR measurements on magnetically oriented microcrystal suspensions (MOMS).
- Employed modulated rotation of the static magnetic field or sample tube to align microcrystals.
- Developed a probe for applying an elliptically rotating magnetic field and obtained SC rotation patterns via solid-state CP NMR.
Main Results:
- Successfully obtained three-dimensional MOMS (3D-MOMS) by aligning microcrystals in a viscous medium.
- Achieved SC rotation patterns from 3D-MOMS without the need for elaborate reference frame adjustments.
- Monitored spectral changes during continuous modulated sample rotation to study the 3D magnetic alignment process.
Conclusions:
- The 3D-MOMS approach offers a simplified alternative to traditional SC NMR techniques.
- This method facilitates detailed structural investigations of microcrystalline materials using solid-state NMR.
- The technique provides a more accessible route to obtaining valuable structural information from challenging samples.
Keywords:
Chemical shift anisotropyIn situ measurementMagnetically oriented microcrystal suspension (MOMS)Single-crystal rotation patternMore Related Videos
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