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.
The sensitivity of magnetic resonance force microscopy
(MRFM) is
limited by surface noise. Coating a thin-film polymer sample with
metal has been shown to decrease, by orders of magnitude, sample-related
force noise and frequency noise in MRFM experiments. Using both MRFM
and inductively detected measurements of electron-spin resonance,
we show that thermally evaporating a 12 nm gold layer on a
40 nm nitroxide-doped polystyrene film inactivates the nitroxide
spin labels to a depth of 20 nm, making single-spin measurements
difficult or impossible. We introduce a “laminated sample”
protocol in which the gold layer is first evaporated on a sacrificial
polymer. The sample is deposited on the room-temperature gold layer,
removed using solvent lift-off, and placed manually on a coplanar
waveguide. Electron spin resonance (ESR) of such a laminated sample
was detected via MRFM at cryogenic temperatures using
a high-compliance cantilever with an integrated 100-nm-scale cobalt
tip. A 20-fold increase of spin signal was observed relative to a
thin-film sample prepared instead with an evaporated metal coating.
The observed signal is still somewhat smaller than expected, and we
discuss possible remaining sources of signal loss.
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