4.3 Article

Frequency-agile gyrotron for electron decoupling and pulsed dynamic nuclear polarization

Journal

JOURNAL OF MAGNETIC RESONANCE
Volume 289, Issue -, Pages 45-54

Publisher

ACADEMIC PRESS INC ELSEVIER SCIENCE
DOI: 10.1016/j.jmr.2018.02.010

Keywords

Dynamic nuclear polarization; Electron decoupling; Gyrotron; Chirp pulses; Pulsed DNP

Funding

  1. NSF-IDBR (CAREER) [DBI-1553577]
  2. NIH Director's New Innovator Award from the National Institutes of Health [DP2GM119131]
  3. Small Business Technology Transfer (STTR) grant by the National Science Foundation [STTR 1521314]
  4. Deutsche Forschungsgemeinschaft (DFG) through Emmy Noether grant [C0802/2-1]
  5. BMRZ
  6. DFG (Heisenberg Program and Priority Program) [SPP-1601]
  7. VolkswagenStiftung within Integration of Molecular Components in Functional Macroscopic Systems
  8. Icelandic Research Fund [141062051]
  9. Direct For Biological Sciences
  10. Div Of Biological Infrastructure [1553577] Funding Source: National Science Foundation

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We describe a frequency-agile gyrotron which can generate frequency-chirped microwave pulses. An arbitrary waveform generator (AWG) within the NMR spectrometer controls the microwave frequency, enabling synchronized pulsed control of both electron and nuclear spins. We demonstrate that the acceleration of emitted electrons, and thus the microwave frequency, can be quickly changed by varying the anode voltage. This strategy results in much faster frequency response than can be achieved by changing the potential of the electron emitter, and does not require a custom triode electron gun. The gyrotron frequency can be swept with a rate of 20 MHz/mu s over a 670 MHz bandwidth in a static magnetic field. We have already implemented time-domain electron decoupling with dynamic nuclear polarization (DNP) magic angle spinning (MAS) with this device. In this contribution, we show frequency-swept DNP enhancement profiles recorded without changing the NMR magnet or probe. The profile of endofullerenes exhibits a DNP profile with a <10 MHz linewidth, indicating that the device also has sufficient frequency stability, and therefore phase stability, to implement pulsed DNP mechanisms such as the frequency-swept solid effect. We describe schematics of the mechanical and vacuum construction of the device which includes a novel flanged sapphire window assembly. Finally, we discuss how commercially available continuous-wave gyrotrons can potentially be converted into similar frequency-agile high-power microwave sources. (C) 2018 Published by Elsevier Inc.

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