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Diamond rotors for high magic angle spinning frequencies

Schaffer, Lauren ; Preiss, David ; Palani, Ravi Shankar ; Wiesner, Nicholas ; Liu, Jiaming ; Strymish, Samuel ; Bahri, Salima ; Linse, Sara LU ; Gershenfeld, Neil and Griffin, Robert G. (2025) In Journal of Magnetic Resonance 379.
Abstract

Magic Angle Spinning (MAS) nuclear magnetic resonance (NMR) spectroscopy is limited in spectral resolution by the spinning frequency of rotors that hold the analyte. Traditional yttria-stabilized zirconia (YSZ) rotors have mechanical constraints that typically limit spinning frequencies of 0.7 mm rotors to ωr/2π ∼ 110 kHz. These frequencies are not sufficient to achieve resolution comparable to that of solution NMR, which theoretically requires ωr/2π > 300 kHz. Building upon prior work that utilized rotary-assisted drilling, we present significant advances in diamond rotor fabrication using a high precision lathe and a centerless laser machining fixture that achieves improved concentricity of the rotor outer and... (More)

Magic Angle Spinning (MAS) nuclear magnetic resonance (NMR) spectroscopy is limited in spectral resolution by the spinning frequency of rotors that hold the analyte. Traditional yttria-stabilized zirconia (YSZ) rotors have mechanical constraints that typically limit spinning frequencies of 0.7 mm rotors to ωr/2π ∼ 110 kHz. These frequencies are not sufficient to achieve resolution comparable to that of solution NMR, which theoretically requires ωr/2π > 300 kHz. Building upon prior work that utilized rotary-assisted drilling, we present significant advances in diamond rotor fabrication using a high precision lathe and a centerless laser machining fixture that achieves improved concentricity of the rotor outer and inner diameters and spinning stability. The new crop of diamond rotors, which interface with the Bruker MAS 3 spinning system equivalently or better than commercial rotors, were spun using automatic 0.7 mm profiles. Furthermore, diamond rotors can be emptied and repacked, and we describe a set of 3D-printed centrifuge tools for efficient execution of this process. We evaluate chemical vapor deposition (CVD) versus high-pressure high-temperature (HPHT) diamonds as rotor material and find HPHT preferable. Extended spin stability tests and multidimensional NMR spectra of Aβ1–40 demonstrate the robustness and usability of these rotors. These advances pave the way for higher frequency spinning with helium gas in the future, enabling transformative improvements in MAS NMR for biological and material sciences.

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type
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publication status
published
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in
Journal of Magnetic Resonance
volume
379
article number
107909
publisher
Academic Press
external identifiers
  • pmid:40628077
  • scopus:105009906802
ISSN
1090-7807
DOI
10.1016/j.jmr.2025.107909
language
English
LU publication?
yes
id
1ecb339f-b1cb-4568-85f3-9586cf0076b1
date added to LUP
2025-10-31 10:36:39
date last changed
2025-10-31 10:37:04
@article{1ecb339f-b1cb-4568-85f3-9586cf0076b1,
  abstract     = {{<p>Magic Angle Spinning (MAS) nuclear magnetic resonance (NMR) spectroscopy is limited in spectral resolution by the spinning frequency of rotors that hold the analyte. Traditional yttria-stabilized zirconia (YSZ) rotors have mechanical constraints that typically limit spinning frequencies of 0.7 mm rotors to ω<sub>r</sub>/2π ∼ 110 kHz. These frequencies are not sufficient to achieve resolution comparable to that of solution NMR, which theoretically requires ω<sub>r</sub>/2π &gt; 300 kHz. Building upon prior work that utilized rotary-assisted drilling, we present significant advances in diamond rotor fabrication using a high precision lathe and a centerless laser machining fixture that achieves improved concentricity of the rotor outer and inner diameters and spinning stability. The new crop of diamond rotors, which interface with the Bruker MAS 3 spinning system equivalently or better than commercial rotors, were spun using automatic 0.7 mm profiles. Furthermore, diamond rotors can be emptied and repacked, and we describe a set of 3D-printed centrifuge tools for efficient execution of this process. We evaluate chemical vapor deposition (CVD) versus high-pressure high-temperature (HPHT) diamonds as rotor material and find HPHT preferable. Extended spin stability tests and multidimensional NMR spectra of Aβ<sub>1</sub><sub>–</sub><sub>40</sub> demonstrate the robustness and usability of these rotors. These advances pave the way for higher frequency spinning with helium gas in the future, enabling transformative improvements in MAS NMR for biological and material sciences.</p>}},
  author       = {{Schaffer, Lauren and Preiss, David and Palani, Ravi Shankar and Wiesner, Nicholas and Liu, Jiaming and Strymish, Samuel and Bahri, Salima and Linse, Sara and Gershenfeld, Neil and Griffin, Robert G.}},
  issn         = {{1090-7807}},
  language     = {{eng}},
  publisher    = {{Academic Press}},
  series       = {{Journal of Magnetic Resonance}},
  title        = {{Diamond rotors for high magic angle spinning frequencies}},
  url          = {{http://dx.doi.org/10.1016/j.jmr.2025.107909}},
  doi          = {{10.1016/j.jmr.2025.107909}},
  volume       = {{379}},
  year         = {{2025}},
}