We report achieving enhanced nuclear magnetization in a magnetic resonance force microscope experiment at 0.6 tesla and 4.2 kelvin using the dynamic nuclear polarization (DNP) effect. In our experiments a microwire coplanar waveguide delivered radiowaves to excite nuclear spins and microwaves to excite electron spins in a 250 nm thick nitroxide-doped polystyrene sample. Both electron and proton spin resonance were observed as a change in the mechanical resonance frequency of a nearby cantilever having a micron-scale nickel tip. NMR signal, not observable from Curie-law magnetization at 0.6 T, became observable when microwave irradiation was applied to saturate the electron spins. The resulting NMR signal’s size, buildup time, dependence on microwave power, and dependence on irradiation frequency was consistent with a transfer of magnetization from electron spins to nuclear spins. Due to the presence of an inhomogenous magnetic field introduced by the cantilever’s magnetic tip, the electron spins in the sample were saturated in a microwave-resonant slice 10’s of nm thick. The spatial distribution of the nuclear polarization enhancement factor ε was mapped by varying the frequency of the applied radiowaves. The observed enhancement factor was zero for spins in the center of the resonant slice, was ε = +10 to +20 for spins proximal to the magnet, and was ε = −10 to −20 for spins distal to the magnet. We show that this bipolar nuclear magnetization profile is consistent with cross-effect DNP in a ~105 Tm−1 magnetic field gradient. Potential challenges associated with generating and using DNP-enhanced nuclear magnetization in a nanometer-resolution magnetic resonance imaging experiment are elucidated and discussed.

Aligning a microcantilever to an area of interest on a sample is a critical step in many scanning probe microscopy experiments, particularly those carried out on devices and rare, precious samples. We report a series of protocols that rapidly and reproducibly align a high-compliance microcantilever to a <10 μm sample feature under high vacuum and at cryogenic temperatures. The first set of protocols, applicable to a cantilever oscillating parallel to the sample surface, involve monitoring the cantilever resonance frequency while laterally scanning the tip to map the sample substrate through electrostatic interactions of the substrate with the cantilever. We demonstrate that when operating a cantilever a few micrometers from the sample surface, large shifts in the cantilever resonance frequency are present near the edges of a voltage-biased sample electrode. Surprisingly, these "edge-finder" frequency shifts are retained when the electrode is coated with a polymer film and a ∼10 nm thick metallic ground plane. The second series of methods, applicable to any scanning probe microscopy experiment, integrate a single-optical fiber to image line scans of the sample surface. The microscope modifications required for these methods are straightforward to implement, provide reliable micrometer-scale positioning, and decrease the experimental setup time from days to hours in a vacuum, cryogenic magnetic resonance force microscope.

Correction for ‘Dynamic nuclear polarization in a magnetic resonance force microscope experiment’ by Corinne E. Isaac et al., Phys. Chem. Chem. Phys., 2016, 18, 8806–8819.