Bhushan B. Nanotribology and Nanomechanics: An Introduction
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5
Low-Temperature Scanning Probe Microscopy
Markus Morgenstern, Alexander Schwarz, and Udo D. Schwarz
Summary. This chapter is dedicated to scanning probe microscopy (SPM) operated at cryo-
genic temperatures, where the more fundamental aspects of phenomena important in the field
of nanotechnology can be investigated with high sensitivity under well defined conditions.
In general, scanning probe techniques allow the measurement of physical properties down to
the nanometer scale. Some techniques, such as the scanning tunneling microscope and the
scanning force microscope even go down to the atomic scale. Various properties are acces-
sible. Most importantly, one can image the arrangement of atoms on conducting surfaces by
scanning tunneling microscopy and on insulating substrates by scanning force microscopy.
But the arrangement of electrons (scanning tunneling spectroscopy), the force interaction
between different atoms (scanning force spectroscopy), magnetic domains (magnetic force
microscopy), the local capacitance (scanning capacitance microscopy), the local temperature
(scanning thermo microscopy), and local light-induced excitations (scanning near-field mi-
croscopy) can also be measured with high spatial resolution. In addition, some techniques
even allow the manipulation of atomic configurations.
Probably the most important advantage of the low-temperature operation of scanning
probe techniques is that they lead to a significantly better signal-to-noise ratio than meas-
uring at room temperature. This is why many researchers work below 100 K. However, there
are also physical reasons to use low-temperature equipment. For example, the manipulation
of atoms or scanning tunneling spectroscopy with high energy resolution can only be real-
ized at low temperatures. Moreover, some physical effects such as superconductivity or the
Kondo effect are restricted to low temperatures. Here, we describe the design criteria of low-
temperature scanning probe equipment and summarize some of the most spectacular results
achieved since the invention of the method about 20 years ago. We first focus on the scan-
ning tunneling microscope, giving examples of atomic manipulation and the analysis of elec-
tronic properties in different material arrangements. Afterwards, we describe results obtained
by scanning force microscopy, showing atomic-scale imaging on insulators, as well as force
spectroscopy analysis. Finally, the magnetic force microscope, which images domain patterns
in ferromagnets and vortex patterns in superconductors, is discussed. Although this list is far
from complete, we feel that it gives an adequate impression of the fascinating possibilities of
low-temperature scanning probe instruments.
In this chapter low temperatures are defined as lower than about 100 K and are normally
achieved by cooling with liquid nitrogen or liquid helium. Applications in which SPMs are
operated close to 0
◦
C are not covered in this chapter.
180 Markus Morgenstern et al.
5.1 Introduction
More than two decades ago, the first design of an experimental setup was presented
where a sharp tip was systematically scanned over a sample surface in order to ob-
tain local information on the tip-sample interaction down to the atomic scale. This
original instrument used the tunneling current between a conducting tip and a con-
ducting sample as a feedback signal and was named scanning tunneling microscope
accordingly [1]. Soon after this historic breakthrough, it became widely recognized
that virtually any type of tip-sample interaction can be used to obtain local informa-
tion onthe sample by applyingthe same generalprinciple, providedthat the selected
interaction was reasonably short-ranged. Thus, a whole variety of new methods has
been introduced, which are denoted collectively as scanning probe methods.An
overview is given by Wiesendanger [2].
The various methods, especially the above mentioned scanning tunneling mi-
croscopy (STM) and scanning force microscopy (SFM) – which is often further
classified into subdisciplines such as the topography-reflecting atomic force mi-
croscopy (AFM), the magnetic force microscopy (MFM), or the electrostatic force
microscopy (EFM) – have been established as standard methods for surface char-
acterization on the nanometer scale. The reason is that they feature extremely high
resolution (often down to the atomic scale for STM and AFM), despite a principally
simple, compact, and comparatively inexpensive design.
Asideeffect of the simple working principle and the compact design of many
scanning probe microscopes (SPMs) is that they can be adapted to different envi-
ronments such as air, all kinds of gaseous atmospheres, liquids, or vacuum with rea-
sonable effort. Another advantage is their ability to work within a wide temperature
range. A microscope operation at higher temperatures is chosen to study surface
diffusion, surface reactivity, surface reconstructions that only manifest at elevated
temperatures, high-temperature phase transitions, or to simulate conditions as they
occur, e.g., in engines, catalytic converters, or reactors. Ultimately, the upper limit
for the operation of an SPM is determined by the stability of the sample, but thermal
drift, which limits the ability to move the tip in a controlled manner over the sample,
as well as the depolarization temperature of the piezoelectric positioning elements
might further restrict successful measurements.
On the other hand, low-temperature (LT) application of SPMs is much more
widespread than operation at high temperatures. Essentially five reasons make re-
searchers adapt their experimental setups to low-temperature compatibility. These
are: (1) the reduced thermal drift, (2) lower noise levels, (3) enhanced stability of tip
and sample, (4) the reduction in piezo hysteresis/creep, and (5) probably the most
obvious, the fact that many physical effects are restricted to low temperature. Rea-
sons (1) to (4) only apply unconditionally if the whole microscope body is kept at
low temperature (typically in or attached to a bath cryostat, see Sect. 5.3). Setups
in which only the sample is cooled may show considerably less favorable operating
characteristics. As a result of (1) to (4), ultrahigh resolution and long-term stability
can be achieved on a level that significantly exceeds what can be accomplished at
5 Low-Temperature Scanning Probe Microscopy 181
room temperature even under the most favorable circumstances. Typical examples
for (5) are superconductivity [3] and the Kondo effect [4].
5.2 Microscope Operation at Low Temperatures
Nevertheless, before we devote ourselves to a short overview of experimental LT-
SPM work, we will take a closer look at the specifics of microscope operation at
low temperatures, including a discussion of the correspondinginstrumentation.
5.2.1 Drift
Thermal drift originates from thermally activated movements of the individual
atoms, which are reflected by the thermal expansion coefficient. At room temper-
ature, typical values for solids are on the order of (1−50)×10
−6
K
−1
.Ifthetemper-
ature could be kept precisely constant, any thermal drift would vanish, regardless
of the absolute temperature of the system. The close coupling of the microscope to
a large temperature bath that maintains a constant temperature ensures a significant
reduction in thermal drift and allows for distortion-free long-term measurements.
Microscopes that are efficiently attached to sufficiently large bath cryostats, there-
fore, show a one- to two-order-of-magnitude increase in thermal stability compared
with non-stabilized set-ups operated at room temperature.
A second effect also helps suppress thermally induced drift of the probing tip
relative to a specific location on the sample surface. The thermal expansion coeffi-
cients at liquid-helium temperatures are two or more orders of magnitude smaller
than at room temperature. Consequently, the thermal drift during low-temperature
operation decreases accordingly.
For some specific scanning probe methods, there may be additional ways in
which a change in temperature can affect the quality of the data. In frequency-
modulation SFM (FM-SFM), for example, the measurement principle relies on the
accurate determination of the eigenfrequency of the cantilever, which is determined
by its spring constant and its effective mass. However, the spring constant changes
with temperature due to both thermal expansion (i.e., the resulting change in the
cantilever dimensions) and the variation of the Young’s modulus with temperature.
Assuming drift rates of about 2mK/min, as is typical for room-temperature meas-
urements, this effect might have a significant influence on the obtained data.
5.2.2 Noise
The theoretically achievableresolution in SPM often increaseswith decreasingtem-
perature due to a decrease in thermally induced noise. An example is the thermal
noise in SFM, which is proportional to the square root of the temperature [5, 6].
Lowering the temperature from T = 300 K to T = 10K thus results in a reduction of
the thermal frequency noise by more than a factor of five. Graphite, e.g., has been