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High-resolution nanoscale NMR for arbitrary magnetic fields

MetadataDetails
Publication Date2023-10-17
JournalCommunications Physics
AuthorsJonas Meinel, Minsik Kwon, R. Maier, Durga Bhaktavatsala Rao Dasari, Hitoshi Sumiya
InstitutionsMax Planck Institute for Solid State Research, University of Stuttgart
Citations9
AnalysisFull AI Review Included
  • Core Innovation: Introduction of an Electron Nuclear Double Resonance Quantum Heterodyne (ENDOR Qdyne) protocol enabling high-resolution nanoscale Nuclear Magnetic Resonance (NMR) spectroscopy applicable at arbitrary (including high) magnetic fields.
  • High-Field Capability: The method eliminates the need for microwave (MW) π-pulses faster than the nuclear Larmor frequency (a requirement for conventional Qdyne), allowing extension to high fields (e.g., 8 T) where chemical shift resolution is maximized.
  • Spectral Resolution: Demonstrated a spectral resolution (decay rate Γ) of 0.6 ± 0.1 kHz on a single weakly coupled 13C nuclear spin (Azz = 6 kHz).
  • Performance Comparison: The ENDOR Qdyne decay rate (0.6 kHz) was significantly better than the conventional Dynamical Decoupling (DD)-based Qdyne protocol (1.4 ± 0.3 kHz) measured on the same spin.
  • Decoherence Mechanism Identified: The primary linewidth-limiting decoherence source was identified as the combination of NV-spin-initialization infidelity ($f \approx 0.9$) and strong sensor-target coupling (Azz).
  • Future Resolution Potential: Theoretical prediction suggests achieving a 1 Hz linewidth for 1H target spins at an NV depth of 4.2 nm.
  • Mechanism: Transverse nuclear spin polarization (Ix, Iy) is converted to longitudinal polarization (Iz) using phase-coherent Radio Frequency (RF) pulses, which is then sensed via the static hyperfine interaction (SzIz) using a Ramsey sequence.
ParameterValueUnitContext
Magnetic Field (B)0.25TProof-of-principle experiment (moderate field)
Target NucleusSingle 13CSpin-1/2Weakly coupled to NV center
Hyperfine Coupling (Azz)6kHzFor the demonstrated 13C spin
13C Larmor Frequency2.336 ± 0.018kHzMeasured via ENDOR Qdyne
ENDOR Qdyne Decay Rate (Γ)0.6 ± 0.1kHzMeasured on 13C (Azz = 6 kHz)
Conventional Qdyne Decay Rate (Γ)1.4 ± 0.3kHzMeasured on same 13C spin
Lowest Observed Linewidth27 ± 9HzObserved for NV-13C pairs with Azz < 70 Hz
Required MW Pulse Length (Conventional)< 8nsRequired for 120 MHz proton Larmor (3 T field)
NV Electron T2* Lifetime50”sTypical lifetime in the 12C-enriched diamond
NV Electron T2 Lifetime≈ 300”sTypical lifetime in the 12C-enriched diamond
NV Initialization Fidelity ($f$)≈ 0.9DimensionlessUsed in decoherence modeling
Diamond Enrichment99.995%12C enrichment
Electron Irradiation Fluence1.3 x 1011cm-2Used for NV creation (2 MeV electrons)
Annealing Temperature1000°CPost-irradiation annealing (2 h in vacuum)
Predicted 1H Linewidth (Goal)1HzPredicted at NV depth (dNV) of 4.2 nm

The experiment utilizes a confocal room-temperature single NV setup combined with arbitrary waveform generators for precise spin control.

  • Material: (111)-oriented polished diamond slice (2 mm x 2 mm x 80 ”m).
  • Growth: High-pressure high-temperature (HPHT) method (5.5 GPa, 1350 °C) using high-purity Fe-Co-Ti solvent and 12C-enriched solid carbon.
  • NV Generation: Intrinsic nitrogen was used. Irradiation performed with 2 MeV electrons at room temperature, total fluence 1.3 x 1011 cm-2.
  • Post-Processing: Annealed at 1000 °C for 2 hours in vacuum.

2. ENDOR Qdyne Protocol (Coherent Sequential Double Resonance)

Section titled “2. ENDOR Qdyne Protocol (Coherent Sequential Double Resonance)”

The protocol combines ENDOR methods with quantum heterodyne measurements to sample nuclear precession phase coherently across multiple electron spin detection runs.

StepActionPurpose / Mechanism
InitializationOptical excitation (520 nm laser)Initializes NV electron spin into ms = 0 state.
Nuclear PolarizationPulse-pol sequenceHyperpolarizes the target 13C nuclear spin.
Precession Start(π/2)ref RF pulsePrepares the nuclear spin in the superposition state (e.g., |+y>).
Free Evolution (Tfid)Nuclear spin precesses freelyAcquires phase (ΔωTfid) relative to the coherent RF source.
Phase Mapping (Ix → Iz)(3π/2)ref+Ί RF pulseRotates the nuclear spin polarization from the transverse plane (Ix, Iy) to the measurement basis (Iz).
Sensing Block (Tsens)Ramsey sequence on NV spinMaps the nuclear Iz polarization onto the NV electron spin (Sz) via the static hyperfine interaction (AzzSzIz).
ReadoutLaser pulseOptically reads out the NV electron spin state (Sz).
Back Rotation (Iz → Ix)(π/2)ref+Ί RF pulseRotates the nuclear spin back into the transverse plane to continue free evolution.
RepetitionProtocol repeated M timesSamples the nuclear oscillation phase coherently.
Industry / FieldApplicationRelevance to ENDOR Qdyne
Nanoscale NMR SpectroscopyHigh-resolution chemical analysis of ultra-small samples (micro- to nanoscales).Enables chemical shift and J-coupling resolution by operating at high magnetic fields (e.g., 8 T).
Quantum SensingDevelopment of robust, high-fidelity quantum sensors based on NV centers.Overcomes the fundamental T1 limit of the sensor spin, enhancing spectral resolution beyond conventional limits.
Structural Biology / ChemistryNMR study of proteins, short-lived molecules, and molecular dynamics in confined volumes.High-field capability increases thermal polarization and sensitivity, reducing the required sensing volume.
Solid-State PhysicsCharacterization of nuclear spin baths and hyperfine dynamics in diamond and other host materials.Provides a method to study decoherence mechanisms (like initialization infidelity) in detail across varying coupling strengths (Azz).
Advanced Materials CharacterizationSurface NMR experiments on diamond or other materials where target nuclei are weakly coupled and distant from the sensor.ENDOR Qdyne is advantageous for sensing distant ensembles of weakly coupled nuclear spins, crucial for surface NMR.
View Original Abstract

Abstract Nitrogen vacancy (NV) centers are a major platform for the detection of nuclear magnetic resonance (NMR) signals at the nanoscale. To overcome the intrinsic electron spin lifetime limit in spectral resolution, a heterodyne detection approach is widely used. However, application of this technique at high magnetic fields is yet an unsolved problem. Here, we introduce a heterodyne detection method utilizing a series of phase coherent electron nuclear double resonance sensing blocks, thus eliminating the numerous Rabi microwave pulses required in the detection. Our detection protocol can be extended to high magnetic fields, allowing chemical shift resolution in NMR experiments. We demonstrate this principle on a weakly coupled 13 C nuclear spin in the bath surrounding single NV centers, and compare the results to existing heterodyne protocols. Additionally, we identify the combination of NV-spin-initialization infidelity and strong sensor-target-coupling as linewidth-limiting decoherence source, paving the way towards high-field heterodyne NMR protocols with chemical resolution.