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Wide-Field Dynamic Magnetic Microscopy Using Double-Double Quantum Driving of a Diamond Defect Ensemble

MetadataDetails
Publication Date2021-05-14
JournalPhysical Review Applied
AuthorsZeeshawn Kazi, Isaac M. Shelby, Hideyuki Watanabe, Kohei M. Itoh, V. Shutthanandan
InstitutionsNational Institute of Advanced Industrial Science and Technology, Keio University
Citations25
AnalysisFull AI Review Included

The research introduces the Double-Double Quantum (DDQ) driving technique to significantly enhance the performance of wide-field Nitrogen Vacancy (NV) ensemble magnetic microscopy for dynamic applications.

  • Core Innovation: DDQ driving utilizes a four-tone Radio Frequency (RF) pulse sequence to suppress spurious contrast generated by pixel-to-pixel variations in the NV resonance curve shape (specifically, optical contrast $C$ and linewidth $\delta\nu$).
  • Performance Enhancement: DDQ successfully mitigates non-magnetic gradients (strain, temperature, electric field) and eliminates the dominant source of imaging noise caused by inhomogeneous broadening in state-of-the-art NV surfaces.
  • Dynamic Capability: The technique enables high-frame-rate imaging (demonstrated at 15.6 Hz) of time-dependent magnetic fields, a capability previously limited by the slow acquisition required for full resonance curve fitting.
  • Sensitivity: The sensor platform achieved an average volume-normalized DC magnetic sensitivity of 31 nT Hz-1/2 ”m3/2.
  • Application Proof: DDQ was used to image the dynamic reorientation of a single ferromagnetic nanoparticle tethered by a DNA molecule, demonstrating its efficacy for micron-scale dynamic magnetometry in single-molecule biophysics.
  • Operational Simplicity: The DDQ method requires only a two-image sequence and no phase control of the RF excitation, simplifying implementation compared to other quantum control schemes.
ParameterValueUnitContext
NV Layer Thickness150nm15N doped layer grown by CVD
Substrate Purity99.999%12C electronic-grade diamond substrate
Implantation Species/EnergyHe+ / 25keVUsed for vacancy formation
Implantation Dose5 x 1011ions/cm2Vacancy creation density
NV Ensemble Density1.7 x 1016cm-3Resulting density in the active layer
Spin Coherence Time (T2)2.5”sEnsemble spin coherence time
Volume-Normalized Sensitivity (ηNV)31nT Hz-1/2 ”m3/2Average DC magnetic sensitivity
Optical Excitation Wavelength532nmLaser used for pumping and readout
Optical Pulse Duration500nsPulsed excitation scheme
RF π-Pulse Duration3500nsPulsed RF control
External Static Magnetic Field (Bext)1mTApplied along the (111) NV orientation
15N Hyperfine Splitting3.05MHzSeparation between RF tones
Dynamic Imaging Frame Rate15.6HzAchieved rate (64 ms exposure per frame)
Nanoparticle-Sensor Distance~400nmApproximate distance in the Tethered-Particle-Motion (TPM) assay

The wide-field magnetic particle imaging (magPI) platform relies on precise sensor fabrication and a novel quantum control sequence:

  1. Diamond Sensor Fabrication: A 150 nm thick layer of 15N doped, isotope-purified (99.999% 12C) diamond was grown via Chemical Vapor Deposition (CVD) on an electronic-grade substrate.
  2. Vacancy Creation and Annealing: Vacancies were created using 25 keV He+ implantation (5 x 1011 ions/cm2). The sample underwent a two-step anneal: 900 °C in vacuum (2 hours) for NV formation, followed by 425 °C in O2 (2 hours) for charge state stabilization.
  3. Pulsed ODMR Readout: Optical and RF fields are applied separately in a pulsed sequence (”s-scale) to eliminate optical power broadening. A 532 nm laser pumps the NV ensemble, and emitted photoluminescence (PL) is captured by a sCMOS camera.
  4. RF Excitation Scheme: RF excitation is delivered via a broadband microwave antenna. Each required RF frequency is mixed to create two equal tones separated by 3.05 MHz, simultaneously driving the two 15N-NV hyperfine transitions.
  5. Double-Double Quantum (DDQ) Driving: The DDQ technique employs four distinct RF tones (f1, f2, f3, f4) applied in a two-image sequence.
    • The first image, Ion(f1, f4), uses RF applied at the outer inflection points of the two resonance curves.
    • The second image, Ion(f2, f3), uses RF applied at the inner inflection points.
  6. DDQ Signal Calculation: The DDQ difference image (DI) is calculated as a normalized ratio: DDQ = 2 * [Ion(f1, f4) - Ion(f2, f3)] / [Ion(f1, f4) + Ion(f2, f3)]. This normalization cancels out common-mode shifts and minimizes the dependence on local contrast (C) and linewidth ($\delta\nu$) variations.
  7. Dynamic Imaging Demonstration: The DDQ method was applied to a Tethered-Particle-Motion (TPM) assay, imaging the magnetic field produced by a 500 nm ferromagnetic nanoparticle tethered by a single DNA molecule as it reorients under fluid flow.

The DDQ technique significantly improves the reliability and speed of NV ensemble magnetometry, opening doors for high-performance commercial applications:

  • Biomagnetic Sensing and Diagnostics: High-frame-rate tracking of magnetic labels (nanoparticles) in biological systems, enabling dynamic studies of molecular motors, fluid mechanics, and single-molecule biophysics without complex per-pixel calibration.
  • Spintronics and Materials Science: Wide-field mapping of local magnetic fields and strain in novel magnetic materials, antiferromagnets, and spintronic devices, crucial for quality control and fundamental research.
  • Integrated Circuit (IC) Analysis: Non-invasive, room-temperature magnetic imaging of current flow and magnetic leakage fields in microelectronics, facilitating failure analysis and device characterization at high speeds.
  • Quantum Sensor Development: DDQ provides a robust quantum control method for mitigating fabrication inhomogeneities, leading to more uniform and reliable NV ensemble sensors suitable for large-area commercial deployment.
  • Geomagnetism and Paleomagnetism: High-resolution mapping of magnetic fields in geological samples, where rapid acquisition is necessary to characterize large areas or time-sensitive processes.
View Original Abstract

Wide-field magnetometry can be realized by imaging the optically-detected magnetic resonance of diamond nitrogen vacancy (NV) center ensembles. However, NV ensemble inhomogeneities significantly limit the magnetic-field sensitivity of these measurements. We demonstrate a double-double quantum (DDQ) driving technique to facilitate wide-field magnetic imaging of dynamic magnetic fields at a micron scale. DDQ imaging employs four-tone radio frequency pulses to suppress inhomogeneity-induced variations of the NV resonant response. As a proof-of-principle, we use the DDQ technique to image the dc magnetic field produced by individual magnetic-nanoparticles tethered by single DNA molecules to a diamond sensor surface. This demonstrates the efficacy of the diamond NV ensemble system in high-frame-rate magnetic microscopy, as well as single-molecule biophysics applications.