Useful Things for the Lab
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1 Recipes
for successful
tip-scattering scanning probe microscopy
1.1 Signal assignment
One of the major challenges in
scattering-type near-field microscopy is
the proper signal assignment. That involves in particular the unique
distinction between the
true near-field process, the far-field background, and topographic and
other
effects. The signals emerging from the spatially localized
optical tip-sample interaction and the other scattering and emission
channels are in most cases indistinguishable a
priori . This
gives rise to a variety of possible imaging artefacts where the
apparent
contrast, e.g., in the simplest case, is due to interference effects as
a result of topographic height variations. Yet, even for planar
surfaces several artefacts are possible, with 3D spatial variations
in the dielectric function of the sample material being the most
prominent one.
Careful spectroscopic measurements, variations of tip-sample
distance, and control experiments with suitable reference
samples
can help to identify the signal sources. For details please see our
corresponding publications and those of other groups on that subject.
1.2 Tip
preparation
A practical challenge concerns the
preparation of suitable tips that
"work", i.e., provide sufficient field enhancement and spatial
localization for high resolution and sensitive tip-scattered near-field
experiments. While a sharp tip apex is of highest importance, a
consistent taper and smooth surface are also correlated with
sensitivity in near field experiments. Through an electrochemical
etching procedure, we can reproducibly fabricate Au tips with suitable
features and apex radii of < 20 nm.
This is accomplished by the electrochemical dissolution of Au wire in a
1:1 solution of concentrated HCl:Ethanol. When a potential of ~2.2 V is
applied to a gold wire immersed in such a solution with respect to a Pt
ring electrode, etching occurs at an increased rate near the meniscus
of the solution. The etching will continue in this region until the
lower portion detaches. The remaining portion of the wire is then used
as a scanning probe tip. However, if the voltage continues to be
applied to the Au wire, etching will continue, resulting in blunted
tips. In order to prevent this, we use a fast cut-off circuit to remove
the applied potential upon the detachment of the lower wire.
The details of the etching process are complex with several parameters
influencing the details of the resulting tip geometry. We have been
able to refine the technique by monitoring the
current during the etching procedure. Periodic current oscillations are
observed during this procedure due to the cyclic depletion and
replenishing of the local electrolyte concentration at the wire. A good
periodicity of the current oscillations is strongly
indicative of
a consistent taper as well as smooth surface. Furthermore, this is
suitable for the determination of an optimum etching voltage.
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Schematic
of the etching setup. a) A Au wire is immersed into a 1:1 solution of
concentrated HCl:Ethanol. A voltage of 2.2 V is applied at the wire
with respect to a Pt cathode. The etching is monitored with a CCD
camera. b) Etching proceeds near the meniscus of the solution until the
lower portion of the wire detaches and the upper portion is used as
the tip. c) the etching current during the process exhibits periodic
oscillations which decrease in frequency in the later stages. A good
periodicity is indicative of a homogeneous taper and smooth surface and
is a suitable criterion for establishing the etching voltage. |
Etching References:
C. C. Neacsu, G. A. Reider and M. B. Raschke, Phys. Rev. B, 71:201402
(2005).
Wang et al.,
App. Phys. Lett., 91:101105 (2007).
C. C. Neacsu, S. Berweger and M. B. Raschke, J. Nanobiotechnology (In
Press).