Solid-State NMR Sample Holder for Thin-Film Analysis
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Solution Overview
Problem
Existing solid-state NMR spectroscopy methods for thin-film samples require sample destruction and are unsuitable for high-resolution measurements due to limitations in sample handling, spinning speed, and signal intensity, especially when dealing with large disklike samples that cannot be inserted into ordinary sample tubes.
Innovation Solution
A high-resolution solid-state NMR spectrometer with a disposable sample-holding portion and a surface coil mounted on an RF circuit substrate, allowing for disklike samples to be measured intact by spinning at high speed while maintaining the magic angle, enabling RF pulse irradiation and detection without deforming the sample.
Engineering Contradictions & Design Principles
Engineering Contradiction Analysis
1Ease of manufacture
If a thin-film sample is scraped off from the supporting basic material and loaded into a sample tube for NMR measurement, then the sample can be measured by ordinary solid-state NMR spectrometer, but the film is processed and destroyed, thus compromising the reliability of the obtained data
Solution Approach 1:
The sample holder is divided into a disklike portion for holding the thin-film sample and a cylindrical portion for insertion into the rotor. This segmentation allows the thin-film sample to be held in its original state on the disklike portion while the cylindrical portion interfaces with the NMR spectrometer system, eliminating the need to scrape or process the film.
Solution Approach 2:
The sample holder acts as an intermediary device between the thin-film sample and the NMR measurement system. It provides a bridge that allows the sample to be measured in its original state without direct contact with or processing by the measurement system, thus preserving sample integrity while enabling measurement.
2Quantity of substance
If a large disklike sample that cannot be inserted into an ordinary sample tube is measured, then the sample size is adequate for representation, but the sample cannot be loaded into conventional NMR sample tubes
Solution Approach 1:
The sample holder is divided into a disklike portion for holding the thin-film sample and a cylindrical portion for insertion into the rotor. This segmentation allows the thin-film sample to be held in its original state on the disklike portion while the cylindrical portion interfaces with the NMR spectrometer system, eliminating the need to scrape or process the film.
Solution Approach 2:
The sample holder transitions the sample from a two-dimensional thin-film form to a three-dimensional configuration where the disklike sample is mounted on a cylindrical holder. This dimensional transformation allows the large-area thin-film sample to be accommodated within the constraints of the NMR rotor while maintaining its integrity.
3Measurement precision
If the sample is spun at high speed to achieve high-resolution NMR spectra, then the spectral linewidth is sharpened and chemical shift terms can be extracted, but the sample holder must be securely mounted to the rotor
Solution Approach 1:
The sample holder merges the disklike sample-holding portion with the cylindrical rotor-insertion portion into a single integrated component. This combination ensures that the sample is securely mounted while maintaining the simplicity of the overall structure, allowing high-speed spinning without complex mounting mechanisms.
Solution Approach 2:
The sample holder is designed as a disposable component that can be easily attached to and removed from the rotor. This approach eliminates the need for complex, reusable mounting mechanisms while ensuring secure attachment during high-speed spinning, as the entire holder can be replaced rather than disassembled and reassembled.
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
Enables high-sensitivity, non-destructive, in-situ measurements of thin-film samples at high resolution, reducing experimental time and improving signal intensity, and allowing for the analysis of physical properties without altering the sample's state.
Implementation Method 1
a rotor (34) holding a sample and disposed in the stator, the rotor having a one-end portion in which an engaging mechanism (35) is mounted
Implementation Method 2
spinning the rotor at high speed about an axis tilted at an angle of about 54.7° (i.e., the magic angle) to the static magnetic field
Implementation Method 3
RF excitation pulses are directed at the sample from a transmit coil while spinning the rotor at high speed about an axis tilted at an angle of about 54.7° (i.e., the magic angle) to the static magnetic field
Implementation Method 4
a surface coil (40) mounted on an RF circuit substrate (41)
Data Source
AI summary
A high-resolution solid-state NMR spectrometer which can measure a disklike sample. The spectrometer includes: a stator having an air bearing disposed within the static magnetic field, the rotor being disposed in the stator; and an engaging mechanism mounted in a one-end portion of the rotor and detachably holding a sample holder that holds the disklike sample.