Spherical Rotors for Stable High-Frequency MAS NMR

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Solution Overview

Problem

Conventional cylindrical rotors in nuclear magnetic resonance (NMR) spectroscopy face limitations in spinning frequency, stability, and sample exchange efficiency, particularly in magic angle spinning (MAS) experiments, due to their inherent instability and complex sample handling requirements.

Innovation Solution

The use of spherical rotors with equatorially spaced notches and a stator design that incorporates a single gas stream for spinning, providing bearing, propulsion, and temperature control, allows for stable spinning at higher frequencies and simplified sample exchange, enabling improved NMR signal sensitivity and reduced cryogen usage.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Speed

If conventional cylindrical rotors are used in MAS NMR experiments, then the sample can be spun at certain frequencies, but the spinning stability and maximum frequency are limited due to inherent instability

Engineering Contradiction:
Improvespinning frequencyVSAvoidspinning stability
Core Design Contradiction:
SpeedVSReliability

Solution Approach 1:

The patent replaces the conventional cylindrical rotor shape with a spherical rotor shape. This geometric change from cylinder to sphere fundamentally alters the rotational dynamics, eliminating the instability inherent in cylindrical designs and enabling significantly higher spinning frequencies while maintaining exceptional stability throughout the NMR experiment.

Inventive Principle:
Principle #14Spheroidality (Curvature)

2Ease of operation

If conventional cylindrical rotors with complex sample handling systems are used, then samples can be loaded and exchanged, but the sample exchange efficiency is reduced and handling complexity increases

Engineering Contradiction:
Improvesample exchange efficiencyVSAvoidsample handling complexity
Core Design Contradiction:
Ease of operationVSDevice complexity

Solution Approach 1:

The spherical rotor system divides the sample handling function into separate components: the simple spherical rotor itself and an external sample loading mechanism. This segmentation allows the rotor to be a simple, exchangeable component while the complex loading operations are performed externally, dramatically simplifying the rotor design and improving exchange efficiency.

Inventive Principle:
Principle #1Segmentation

3Speed

If multiple gas streams are used for bearing and propulsion in cylindrical rotors, then the rotor can be spun, but the system complexity and cryogen usage increase

Engineering Contradiction:
Improvespinning capabilityVSAvoidgas stream system complexity
Core Design Contradiction:
SpeedVSDevice complexity

Solution Approach 1:

The spherical rotor design merges the bearing function and propulsion function into a single integrated system. The gas inlet positioned at the pole provides both bearing support and rotational propulsion through the equatorial notch, eliminating the need for separate gas stream systems and significantly reducing overall system complexity.

Inventive Principle:
Principle #5Merging (Combining)

4Measurement precision

If conventional cylindrical rotors are used, then NMR signals can be obtained, but the sensitivity is reduced compared to spherical rotors

Engineering Contradiction:
ImproveNMR signal sensitivityVSAvoidrotor stability
Core Design Contradiction:
Measurement precisionVSStability of the object's composition

Solution Approach 1:

The spherical geometry of the rotor improves NMR signal sensitivity through more efficient spin dynamics and reduced mechanical instability. The spherical shape enables superior magnetic field homogeneity and more stable rotational motion, directly enhancing the quality and sensitivity of the NMR signals obtained from the sample.

Inventive Principle:
Principle #14Spheroidality (Curvature)

Applied Scientific Principles

This section explains which scientific principles are used to turn an abstract innovation direction into a practical engineering solution.

Function Achieved in This Case

Spherical rotors demonstrate enhanced spinning stability and frequency, increased NMR sensitivity, and simplified sample handling, overcoming the limitations of cylindrical rotors in MAS experiments, while reducing the need for extensive cryogenic resources.

Implementation Method 1

a single gas stream for spinning, providing bearing, propulsion, and temperature control

Methodology Applied
Scientific EffectAerodynamic force: Aerofoil

Implementation Method 2

the stator comprises at least one gas inlet and at least one exhaust gas outlet

Methodology Applied
Scientific EffectGas flow: Fluid Spray

Implementation Method 3

spinning the spherical rotor at a frequency ranging from about 0 kHz to about 130 kHz

Methodology Applied
Scientific EffectMagic angle spinning:

Implementation Method 4

spinning the spherical rotor at higher frequencies

Methodology Applied
Scientific EffectCentrifugal force: Centrifugal Force

Implementation Method 5

a single gas stream for spinning, providing bearing, propulsion, and temperature control

Methodology Applied
Scientific EffectConvection: Convection

Data Source

PatentEP3717924B1Spherical rotors and their use in NMR spectroscopy
Publication Date: 2023.10.11 WASHINGTON UNIV IN SAINT LOUIS
  • EP3717924B1 patent drawingFigure 1A~1D
  • EP3717924B1 patent drawingFigure 2A~2B
  • EP3717924B1 patent drawingFigure 3A(i)~3A(ii)

AI summary

Among the various aspects of the present disclosure is the provision of systems and spherical rotors suitable for use in magic angle spinning (MAS) nuclear magnetic resonance (NMR) spectroscopy and methods of use thereof.