Design of a cryogen-free high field dual EPR and DNP probe. 2023

Kan Tagami, and Raymond Thicklin, and Sheetal Jain, and Asif Equbal, and Miranda Li, and Toby Zens, and Anthony Siaw, and Songi Han
Department of Chemistry and Biochemistry, University of California, Santa Barbara, Santa Barbara, CA 93106, United States.

We present the design and construction of a cryogen free, dual electron paramagnetic resonance (EPR) and nuclear magnetic resonance (NMR) probe for novel dynamic nuclear polarization (DNP) experiments and concurrent "in situ" analysis of DNP mechanisms. We focus on the probe design that meets the balance between EPR, NMR, and low temperature performance, while maintaining a high degree of versatility: allowing multi-nuclear NMR detection as well as broadband DNP/EPR excitation/detection. To accomplish high NMR/EPR performance, we implement a novel inductively coupled double resonance NMR circuit (1H-13C) in a solid state probe operating at cryogenic temperatures. The components of the circuit were custom built to provide maximum NMR performance, and the physical layout of this circuit was numerically optimized via magnetic field simulations to allow maximum microwave transmission to the sample for optimal EPR performance. Furthermore this probe is based around a cryogen free gas exchange cryostat and has been designed to allow unlimited experiment times down to 8.5 Kelvin with minimal cost. The affordability of EPR/DNP experiment is an extremely important aspect for broader impact with magnetic resonance measurements. The purpose of this article is to provide as complete information as we have available for others with interest in building a dual DNP/EPR instrument based around a cryogen-free cryostat.

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