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Parallel detection and spatial mapping of large nuclear spin clusters

MetadataDetails
Publication Date2022-03-10
JournalNature Communications
AuthorsK. S. Cujia, Konstantin Herb, Jonathan Zopes, John M. Abendroth, Christian L. Degen
InstitutionsETH Zurich
Citations25
AnalysisFull AI Review Included
  • Core Achievement: Demonstrated parallel detection and three-dimensional (3D) spatial mapping of large nuclear spin clusters (up to 29 13C nuclei) surrounding a single Nitrogen-Vacancy (NV) center in diamond.
  • Single-Molecule MRI Advancement: This strategy fulfills a critical requirement for developing single-molecule Magnetic Resonance Imaging (MRI) by efficiently localizing multiple spins at ambient (room) temperature.
  • Spatial Range: Successfully mapped 13C spins within a 2.4 nm radius. Extrapolation based on electron spin coherence time (T2,e) suggests a potential mapping radius of 5-6 nm for 1H (proton) nuclei.
  • Methodology: The technique combines weak quantum measurements (sampling the Free Induction Decay, FID), phase encoding, and a Generalized Simulated Annealing (GSA) algorithm for robust, parallel extraction of 3D hyperfine parameters.
  • Spatial Selectivity: The protocol is spatially selective, allowing engineers to tune the sensitive slice radius (rslice) by varying the interaction time (tbeta). This avoids interference from strongly-coupled proximal nuclei.
  • Resolution: Statistical analysis confirms that the method achieves sub-Angstrom precision for nuclei located near the maximum sensitivity radius, with volume uncertainties often less than the volume per carbon atom (5.67 A3).
ParameterValueUnitContext
Operating TemperatureAmbientN/ARoom temperature operation, compatible with biological samples.
Nuclear Spin MappedCarbon-13 (13C)N/ANatural isotope abundance (1.1%) in diamond.
Maximum Mapped Radius (13C)2.4nmDemonstrated distance from the NV center.
Extrapolated Radius (1H)5-6nmPotential range for proton detection, limited by T2,e.
NV Center Depth (Tested)~10nmShallow depth, demonstrating compatibility with near-surface sensing.
Electron Spin Coherence Time (T2,e)~50”sMeasured for a 3.5 nm deep NV center.
Bias Magnetic Field (B0)188.89 to 201.29mTExternal field aligned to the NV symmetry axis.
13C Larmor Frequency2.156MHzReference frequency used for spectral calibration.
Number of Spins Mapped (Max)29N/ATotal 13C nuclei successfully localized in one cluster (NV2).
Diamond Lattice Volume per 12C5.67A3Used as a benchmark for single-nucleus resolution.
Spatial Precision (Best Case)< 1AngstromAchieved for 13C spins located near the sensitive slice maximum.
  1. Sample Preparation:

    • Used electronic-grade diamond plates with natural 13C abundance (1.1%).
    • NV centers created via 15N+ ion implantation (5 keV energy) followed by annealing at 850 °C.
    • Nano-pillars etched into the surface to enhance photon collection efficiency.
  2. Spin Control and Setup:

    • NV electronic spins manipulated using microwave pulses (~2.5 GHz) delivered via a coplanar waveguide.
    • Nuclear spins manipulated using broadband radio-frequency (RF) pulses delivered via a planar micro-coil (3 dB bandwidth ~19 MHz).
    • A permanent magnet provided a bias field (B0 ~ 200 mT) aligned to the NV symmetry axis.
  3. Nuclear Hyperpolarization:

    • Nuclear spins were hyperpolarized using a repeated NOVEL (Nuclear spin Orientation via Electron spin Locking) sequence, transferring polarization from the optically-aligned electronic spin.
  4. Weak Measurement Detection Protocol:

    • The Free Induction Decay (FID) signal was acquired by simultaneously exciting all nuclei with a broad-band pi/2 pulse.
    • The transverse nuclear magnetization was sampled using repeated weak measurements, consisting of a Carr-Purcell-Meiboom-Gill (CPMG) pulse train (4-24 pulses) followed by optical readout.
  5. Spatial Selectivity Tuning:

    • The radius of the “sensitive slice” (rslice) was tuned by varying the interaction time (tbeta) of the CPMG sequence.
    • This tuning exploits the balance between signal gain (proportional to hyperfine coupling) and quantum back-action (which causes rapid decay for strongly coupled, proximal spins).
  6. Data Analysis and Localization:

    • Four FID spectra, recorded at different tbeta values, were combined for redundancy and volume coverage.
    • Hyperfine parameters (aparallel, aperpendicular, and phase phi) were extracted by minimizing a total cost function using the Generalized Simulated Annealing (GSA) algorithm.
    • GSA was run on a high-performance cluster to globally optimize the fit parameters (up to 3n + 3 unknowns, where n is the number of spins).
    • 3D spatial locations (r, theta, phi) were calculated by inverting the dipolar hyperfine interaction equation using the extracted hyperfine vector a.
Industry/SectorApplicationTechnical Relevance
Single-Molecule MRIDirect structural determination of individual molecules (proteins, polymers) with 3D resolution and elemental specificity.High spatial resolution (< 5 nm radius potential for 1H) and ambient operating conditions.
Quantum Computing & SimulationCharacterization and calibration of large nuclear spin registers (qubit registers) used in solid-state quantum processors.Provides an efficient tool for mapping the coupling network and cross-talk in multi-qubit systems.
Biotechnology & Drug DiscoveryNanoscale surface NMR for monitoring chemical binding, conformational changes, and surface reactions (e.g., enzyme active sites).Compatibility with near-surface NV centers (< 5 nm depth) and room temperature operation is crucial for biological samples.
Quantum Network NodesMapping the spin environment of central electronic spins used in quantum network nodes and quantum interconnects.Essential for engineering robust, long-coherence quantum memory registers (e.g., 29Si or 13C).
Materials ScienceNanoscale surface NMR spectroscopy for characterizing thin films, deposited molecular layers, and interfaces on diamond substrates.High sensitivity allows detection of weak signals from external spins or dilute surface ensembles.