Utilizing semiconductor nanowires for (opto)electronics requires exact knowledge of their current-voltage properties. We report accurate on-top imaging and I-V characterization of individual as-grown nanowires, using a subnanometer resolution scanning tunneling microscope with no need for additional microscopy tools, thus allowing versatile application. We form Ohmic contacts to InP and InAs nanowires without any sample processing, followed by quantitative measurements of diameter dependent I-V properties with a very small spread in measured values compared to standard techniques.
Utilizing semiconductor nanowires for (opto)electronics requires exact knowledge of their current-voltage properties. We report accurate on-top imaging and I-V characterization of individual as-grown nanowires, using a subnanometer resolution scanning tunneling microscope with no need for additional microscopy tools, thus allowing versatile application. We form Ohmic contacts to InP and InAs nanowires without any sample processing, followed by quantitative measurements of diameter dependent I-V properties with a very small spread in measured values compared to standard techniques.
The development of high-performance/low
cost photovoltaic devices, light-emitting diodes with optimal color-rendering
index, and high-speed/low-power electronics for mobile applications
are three important areas in modern society where novel semiconductor
nanowire structures are expected to lead to qualitative advances in
performance.[1−4] In addition, these new structures are exploratory systems for new
physical phenomena such as Majorana fermions[5,6] and
exciton dynamics.[7,8] Free-standing semiconductor nanowires
in particular offer advantages such as atomically precise heterostructures
in a wide range of materials[9,10] and the epitaxial combination
of III–V semiconductors with Si.[4,11]However,
for the successful realization of future nanowire applications
it is crucial to study how the resistivity and exact I–V behavior of individual nanowires determine the performance of the
entire device. Unfortunately, these parameters cannot be predicted
from known bulk parameters and will depend strongly on the nanowire
surface.[12,13] Even more problematic, most methods that
measure these quantities in a reliable and reproducible fashion in
bulk materials do not work for the nanowire geometry. This has led
to a significant effort to develop specialized methods for characterizing
nanowire electronic properties.[14−18] The most commonly used approach to investigate transport properties
of individual nanowires uses a nanowire field-effect transistor (FET)
geometry where the nanowires are deposited on an insulating substrate
and contacted with metal electrodes defined by electron beam lithography
(EBL).[19,20] There are three significant limitations
with this method. First, the resulting I–V characteristics are often dominated by the contact between the nanowire
and the metal electrodes, rather than the nanowire itself.[21−25] Second, data from broken nanowires in FET geometry are not directly
comparable with nanowire devices in an upright-standing configuration.[26,27] Third, the significant number of processing steps is time-consuming
and strongly limits the versatility of surface treatment and shell
layer design that is inherent to free-standing nanowires.A
more direct concept for measuring single nanowire resistivity
is to establish a point contact between a metallic nanoprobe and the
top end of an upright standing as-grown nanowire. This approach requires
no extra processing, and it provides an epitaxial and therewith well-defined
back contact to the individual nanowire. Talin and co-workers have
recently revealed exciting new insights in transport properties of
nanowires by positioning a W nanoprobe inside a scanning electron
microscope (SEM) for studying the I–V-characteristics
of individual Ge,[28] GaN,[29] InAs,[30] or GaAs[31] nanowires. Comparable investigations have also been reported
by Kavanagh and co-workers for GaAs[32] and
InN[33] nanowires. While these revealed the
device morphology and geometry, the precise structure on top of the
nanowire prior to contacting was not known. Here it should be noted
that the exact structural properties of the contacting area have a
large impact on the results from such contact measurements.[34,35] Alternatively, the nanoprobe can be placed within a transmission
electron microscope (TEM), enabling precise positioning, though under
the nontrivial limitations of the tight TEM geometry and elaborate
sample processing. However, independent realizations of such a setup
found it very challenging,[36,37] if possible at all,[38] to establish an Ohmic contact between the nanowire
and the nanoprobe, which was related to oxidation of the nanoprobe
and to carbon contamination induced by the electron beam.[36] Thus, the main challenges for nanoprobe I–V measurements at single nanowires are (i) the
exact positioning of the nanoprobe toward the nanowire, (ii) to provide
proper surface conditions of both the nanowire and the probe, which
are crucial for establishing a well-defined system, and (iii) to keep
the method versatile.Here, we take the nanoprobe concept a
qualitative step further
and use the scanning tunneling microscope (STM) tip for both imaging
individual upright standing nanowires and for measuring their electrical
properties after establishing a point contact. By performing scanning
tunneling microscopy on upright standing nanowires, which is an unconventional,
though successfully proven geometry,[39] we
completely remove the need for an electron microscope during the measurements.
This setup (i) gives the unique subnanometer resolution of the STM,
(ii) works in an ultrahigh vacuum (UHV) surrounding that implies control
over the surface conditions of sample and probe, and (iii) it can
be realized with only a standard STM and without any sample processing,
being the most direct realization of the nanoprobe concept. We present
first results on homogeneous InP and InAs nanowires where we have
imaged the top end of the nanowires with subnm resolution and routinely
obtained Ohmic contacts between the probe tip and individual nanowires
with a contact resistance of less than 22 Ω. Measured nanowire
resistances R are inversely proportional to the cross-sectional
area for nanowires in a diameter range of 50–170 nm, as expected.
The key prerequisites for the extremely low contact resistance are
oxide-free surfaces enabled by UHV probe treatment and knowledge of
the exact topography on top of the nanowires, since this can significantly
influence the point contact formation.[34] While it might seem surprising that the inherently 2D STM technique
can be used to image structures with such a high aspect ratio as that
of upright standing nanowires, once this conceptual barrier has been
overcome this opens up new radical opportunities in the study of nanowire
devices.All nanowires studied here were grown by molecular
vapor phase
epitaxy (MOVPE).[40] Au nanoparticles were
randomly distributed on the growth substrate using an aerosol technique,
initiating nanowire growth via the vapor–liquid–solid
mode. Trimethylindium ((CH3)3In), phosphine
(PH3), and hydrogen sulfide (H2S) were used
as precursors with molar fractions of 3.5 × 10–6, 6.25 × 10–3, and 2.4 × 10–8 for growing highly S-doped InP nanowires at 420 °C on an n-doped
InP (111)B substrate, as described in more detail in ref (41). InAs nanowires were grown
on an n-doped InAs (111)B substrate using triethylindium ((C2H5)3In) and arsine (AsH3) in two
growth steps: The lower part of the nanowires was Si-doped, while
the upper part remained without intentional doping. After growth,
the nanowire samples were exposed to air during storage until they
were loaded without any further processing or treatment into the UHV
STM chamber. STM measurements were performed in constant current mode
using a JEOL JSTM-4500 XT microscope with an RHK SPM 100 control unit,
bypassed with an external sample voltage supply, and the RHK XPMPro
software. The STM was operated at room temperature at a base pressure
below 10–9 mbar. STM tips were made of 0.25 mm thick
W wire by electrochemical etching in either KOH or NaOH solution,
followed by Ar+ ion sputtering at 2 to 3 keV within the
UHV chamber of the STM. In some cases, the W wire was annealed in
vacuum prior to the etching step, resulting in STM tips with a slightly
higher aspect ratio, which however did not seem to affect the electrical
measurements. I–V spectra of individual contacted
nanowires were acquired using a Stanford Research Systems SR830 Lock-In
Amplifier as a programmable voltage source and a Stanford Research
Systems SR570 Current Preamplifier coupled with a Hewlett-Packard
HP34401A Multimeter, synchronized using a custom written Labview program.(a) The
1 μm × 1 μm STM overview image of upright
standing InAs nanowires, obtained with a sample bias of V = −0.5 V and a tunneling current of I =
100 pA. The actual length of the nanowires is about 2 μm, but
the z position of the STMtip is restricted, so that
it cannot reach down to the substrate. Therefore the color scale of
the STM image corresponds to relative length differences of individual
nanowires, indicated in nm. The inset shows a 3D close-view STM image
of a single nanowire. (b) STM height profile of the nanowire shown
in the inset of (a). Note that the bottom height is determined by
the restricted z range of the STMtip and not by
the sample. The position and diameter of the nanowire and the shape
of the Au particle on top can be obtained with subnm resolution. (c–e)
Sketch of the procedure for measuring the resistivity of individual
nanowires. (c) First, the exact position and shape of a nanowire is
determined by imaging with the STM in top-view geometry. (d) Then,
the STM feedback loop is interrupted and the tip is further approached
toward the nanowire and slightly pushed into the center of the metal
particle on top of the nanowire in a gentle and controlled way, establishing
an Ohmic point contact between the tip and the nanowire. (e) Finally,
an external current preamplifier is connected to measure the I–V properties of the contacted
nanowire.The procedure used here for current–voltage
measurements
of individual semiconductor nanowires is sketched in Figure 1. First, the upright standing nanowires are imaged
by STM, which is a nonconventional and challenging task, that nevertheless
can be realized even with a standard STM. In order not to damage the
nanowires or the probe tip, the STMtip is initially approached toward
the sample in an iterative procedure, until the top end of one or
several nanowires is imaged, as shown in Figure 1a–c. This process is described in more detail in ref (39). For most nanowires studied
here, the nanowire length exceeds the height range of the STM (450
nm), so that the STMtip scans across the top end of the nanowires,
but does not reach the sample surface of the growth substrate. This
results in an STM overview image like the one shown in Figure 1a, where several nanowires exhibit a different height
contrast corresponding to the relative difference in the nanowire
length. It should be noticed that by this approach even a native oxide
layer on the nanowire sample will not affect the STM measurements,
since the STMtip does not reach the oxidized sample substrate but
only the top end of the nanowires, which usually consists of a metal
nanoparticle. One specific nanowire can be chosen for characterization
and a zoomed-in STM image of that nanowire can be taken, as shown
in the inset of Figure 1a. From the STM height
profile displayed in Figure 1b, it can be seen
that the nanowire diameter and the exact topography of its top end
can be obtained with subnanometer resolution. With this information,
the STMtip can be positioned exactly at the center of the upright
standing nanowire, where the point contact has to be established.
Now the constant-current feedback loop of the STM has to be interrupted,
so that the tip can be further approached toward the nanowire until
a point contact is reached (Figure 1d), which
is detected by a sudden increase of the measured current. This current
typically exceeds the saturation limit of the STM electronics, so
that the connection for current read-out is switched to a secondary
current amplifier with a larger range (Figure 1e).
Figure 1
(a) The
1 μm × 1 μm STM overview image of upright
standing InAs nanowires, obtained with a sample bias of V = −0.5 V and a tunneling current of I =
100 pA. The actual length of the nanowires is about 2 μm, but
the z position of the STM tip is restricted, so that
it cannot reach down to the substrate. Therefore the color scale of
the STM image corresponds to relative length differences of individual
nanowires, indicated in nm. The inset shows a 3D close-view STM image
of a single nanowire. (b) STM height profile of the nanowire shown
in the inset of (a). Note that the bottom height is determined by
the restricted z range of the STM tip and not by
the sample. The position and diameter of the nanowire and the shape
of the Au particle on top can be obtained with subnm resolution. (c–e)
Sketch of the procedure for measuring the resistivity of individual
nanowires. (c) First, the exact position and shape of a nanowire is
determined by imaging with the STM in top-view geometry. (d) Then,
the STM feedback loop is interrupted and the tip is further approached
toward the nanowire and slightly pushed into the center of the metal
particle on top of the nanowire in a gentle and controlled way, establishing
an Ohmic point contact between the tip and the nanowire. (e) Finally,
an external current preamplifier is connected to measure the I–V properties of the contacted
nanowire.
Nanowires of different III–V semiconductor materials
like
InP and InAs have been contacted and measured by our method. All nanowires
studied were grown in the particle assisted growth mode using catalytic
Au nanoparticles, which upon growth form Au–In alloys. This
leads to a well-defined situation where a point contact is formed
between the Au–In particle and the STMtip, which is made of
etched tungsten wire and has been sputtered within UHV, meaning that
two clean and completely oxide-free metals are brought into contact.SEM images
of (a) an InP nanowire and (b) an STM probe tip made
of vacuum-annealed W wire after etching in KOH solution and sputtering
using Ar+ ions. The image in (a) was acquired with a tilt angle of
15°. The scale bar is valid for both images.The nanowires studied here had diameters between 50 and 170
nm,
determined by the size of the original Au seed particle, although
the method could well be applied to thinner or thicker nanowires as
well. An SEM image of a typical nanowire can be seen in Figure 2a. The diameters of the nanowires are in the same
range as the width of the STM probe tip, which routinely reaches a
radius of curvature of less than 30 nm, as can be seen in the SEM
image of a typical STMtip shown in Figure 2b. Thus, the process of forming a point contact can be understood
as a sharp, stiff W tip penetrating into the comparably soft, spherical
metal particle on top of the nanowire.
Figure 2
SEM images
of (a) an InP nanowire and (b) an STM probe tip made
of vacuum-annealed W wire after etching in KOH solution and sputtering
using Ar+ ions. The image in (a) was acquired with a tilt angle of
15°. The scale bar is valid for both images.
Formation of an Ohmic
contact between the probe tip and the nanowire:
(a) Change of the measured resistance of four individual nanowires
when the probe tip is gently pushed by small steps into the metal
seed particle on top of the nanowire, as shown schematically in the
inset. Red filled squares, blue open diamonds, green filled circles,
and orange open circles correspond to one of the four nanowires, respectively.
(b–d) I–V curves measured
at one of the nanowires after pushing the tip (b) 1, (c) 4, and (d)
13 steps into the metal particle. The resistance values plotted in
(a) correspond to the averaged slope of the I–V spectra.With the gentle and controlled alignment of the piezo positioners
holding the STMtip, the process of point contact formation can be
monitored, as shown in Figure 3. At the first,
very weak contact between a sharp STMtip and the metal particle on
top of the nanowire, usually a strongly nonlinear I–V spectrum with a very small current in the nanoamperes range is measured,
as shown in Figure 3b. These very small currents
are typical for tunneling through a remaining thin vacuum barrier.
When the tip is pushed slightly further into the metal particle using
nanometer-sized steps, the measured current typically increases with
each step (Figure 3c), until a point where
it increases significantly and the I–V curve
becomes linear (Figure 3d), indicating that
an Ohmic contact has formed. This behavior can be explained by the
geometrical cross-section of the point contact. When the very sharp
tip touches the metal particle at the initial contact, the very small
cross-section does not enable a sufficient current density. With each
small step that the piezo positioner pushes the tip further into the
Au–In particle, the contact cross-section increases and its
resistance decreases, until the cross-section is not limiting the
current flow anymore and an Ohmic contact has formed.
Figure 3
Formation of an Ohmic
contact between the probe tip and the nanowire:
(a) Change of the measured resistance of four individual nanowires
when the probe tip is gently pushed by small steps into the metal
seed particle on top of the nanowire, as shown schematically in the
inset. Red filled squares, blue open diamonds, green filled circles,
and orange open circles correspond to one of the four nanowires, respectively.
(b–d) I–V curves measured
at one of the nanowires after pushing the tip (b) 1, (c) 4, and (d)
13 steps into the metal particle. The resistance values plotted in
(a) correspond to the averaged slope of the I–V spectra.
According
to Figure 3, between 10 and 15
steps by our piezo positioner are typically needed for establishing
an Ohmic contact with a sharp tip. One piezo step corresponds to a
tip movement of about 5 nm if the tip can move freely. This step size
would give an astonishingly large value for the necessary tip-nanowire
positioning. However, we have observed previously that free-standing
nanowires are flexible, even in their axial direction, so that the
attractive electrostatic force between a biased STMtip and a nanowire
can cause the nanowire to stretch several tens of nanometers or by
more than 1% of its length when forming the initial point contact.[39] The nanowire can come back to its initial length
when the STMtip is pushed forward. Thus, we assume that the movement
of the STMtip is mostly compensated by a contracting nanowire, so
that the observed 10 to 15 steps for forming the Ohmic contact probably
correspond to a penetration depth of the tip into the Au–In
particle of around 10 nm. It should be noted that these 10 to 15 steps
are typical for freshly prepared, sharp tips, where the initial point
contact can be assumed to consist of only a few atoms, while rather
blunt tips have been found to form Ohmic contacts already after one
or two steps, which however does not influence the measured I–V properties once the contact has formed. This
behavior confirms that a sufficiently large contact cross-section
is necessary for the Ohmic contact, also in agreement with other nanoprobe
experiments reported in literature.[30] We
note that upon contact, currents up to 30 μA (at 0.1 V) were
measured in a single nanowire. Such high currents might explain the
need for a sufficiently large contact cross-section. On the other
hand, nanowires with Au particle diameters down to 20 nm have successfully
been contacted by this method, giving an upper limit of the necessary
contact cross-section of a few nanometers.After establishing
an Ohmic contact, the tip can be pushed even
further into the metal particle, which will create strain and cause
bending of the nanowire,[36] thereby changing
its intrinsic resistivity. Correspondingly, a very small further decrease
of the measured resistance can be seen in Figure 3 at these conditions. In the following, the slope of the first
linear I–V-curve upon contacting a nanowire
with the STMtip, which usually comes along with a strong increase
of the measured current, will be assigned to be the resistance of
this specific nanowire.[42]Considering
the high currents measured in single nanowires, corresponding
current densities of up to 0.6 × 106 A/cm2 were obtained. This could potentially lead to heating of the device.
We can however repeat I(V) measurements
over time periods varying between minutes and hours and with different
duration of the I(V) measurement
itself with reproducible results. In addition, the effect of carrier
transport on temperature in nanowires has been calculated, indicating
that even for four times as large current densities as used in our
experiments, the temperatures should not go above 250 °C.[43]Measured resistance properties of individual nanowires,
as obtained
from linear I–V-spectra.
(a) Resistance of highly doped InP nanowires. The data in the left
part (triangles) corresponds to as-grown nanowires and the data in
the right part (circles) to nanowires from the same sample after etching
and surface passivation. (b) Resistance of nonintentionally doped
InAs nanowires. The average resistance and standard deviation for
the corresponding nanowires is indicated in (a) and (b). (c) Typical I–V curves of an individual InP
nanowire obtained with the STMtip in point contact (blue, straight
line) and in an FET geometry reference experiment using EBL-defined
contacts (dark green, dotted line). The linear nanowire behavior can
clearly be seen in the STM-based data, while the reference experiment
fails in providing Ohmic contacts. (d) Resistance of the same nanowires
as shown in (a), here plotted over the diameter, which is determined
for each nanowire from the STM images. The experimental uncertainty
of the diameter measurement, mostly due to the convolution with the
STMtip shape, is indicated by error bars. A simple fit of the experimental
data is shown by the green line, confirming the dependence of the
nanowire resistance R on the diameter d with R = 30.3 kΩ nm2/d2.In order to test our
method, we chose to study highly doped nanowires,
where a significant series resistance induced by the contacts would
strongly influence the measured I–V properties.
We used InP nanowires with diameters around 100 nm and lengths of
about 2 μm that were n-doped using H2S.[41] An SEM image of such a nanowire is
shown in Figure 2a. Resistance measurements
on 14 individual nanowires on this sample are presented in the left
part of Figure 4a. All these nanowires showed
linear I–V curves like the one plotted as
blue curve in Figure 4c. The resulting average
resistance was R = 4.3 (±2.2) kΩ.
Figure 4
Measured resistance properties of individual nanowires,
as obtained
from linear I–V-spectra.
(a) Resistance of highly doped InP nanowires. The data in the left
part (triangles) corresponds to as-grown nanowires and the data in
the right part (circles) to nanowires from the same sample after etching
and surface passivation. (b) Resistance of nonintentionally doped
InAs nanowires. The average resistance and standard deviation for
the corresponding nanowires is indicated in (a) and (b). (c) Typical I–V curves of an individual InP
nanowire obtained with the STM tip in point contact (blue, straight
line) and in an FET geometry reference experiment using EBL-defined
contacts (dark green, dotted line). The linear nanowire behavior can
clearly be seen in the STM-based data, while the reference experiment
fails in providing Ohmic contacts. (d) Resistance of the same nanowires
as shown in (a), here plotted over the diameter, which is determined
for each nanowire from the STM images. The experimental uncertainty
of the diameter measurement, mostly due to the convolution with the
STM tip shape, is indicated by error bars. A simple fit of the experimental
data is shown by the green line, confirming the dependence of the
nanowire resistance R on the diameter d with R = 30.3 kΩ nm2/d2.
As a direct comparison, we made several attempts to measure nanowires
from the same sample in the traditional FET configuration. Here the
nanowires were mechanically transferred to a degenerately doped silicon
substrate, which was covered with 100 nm of SiO2 and 10
nm of HfO2. The position of the nanowires was measured
in an optical microscope and after resist deposition contacts were
created to selected nanowires by EBL and metal lift off, using a Ti/Pd
metal combination. However, the observed I–V curves, like the one plotted in green in Figure 4c, were non-Ohmic, and completely dominated by contacts with
Schottky-like barriers. We assume these problems in externally contacting
the nanowires to result from the oxidized nanowire surface, demonstrating
the advantage of our STM-based method for I–V measurements with oxide-free and thus low-resistive contacts.Since the as-grown nanowire sample had been exposed to ambient
air before being transferred into the STM, the measured resistivity
may be influenced by the highly n-doped shell around the nanowire,
for example, an InPO layer.[44] It is well-known that surface chemistry and structure can potentially
influence nanowire properties.[45] In order
to investigate this possibility, we etched the InP nanowire sample
in phosphoric acid and sulfuric acid, followed by surface passivation
using ammonium sulfide,[22] and immediately
transferred them back into the UHV environment of the STM. Resistance
measurements on five individual, freshly etched nanowires are shown
in the right part of Figure 4a, resulting in
an average nanowire resistance of R = 4.2 (±2.5)
kΩ, which is the same value as before the etching procedure.
This indicates that the observed conductance is related to the InP
nanowires themselves and not to the thickness of a shell layer. It
should be noticed, however, that only an almost total removal of the
surface oxides will seriously affect the surface pinning in the case
of InP nanowires, as we have shown before.[44]A significant spread of the measured resistance R among different individual nanowires is observed, as can be seen
in Figure 4a,b. The large spread can be explained
by the variation of the nanowire diameter. From the STM images, which
are taken to characterize a nanowire and its surroundings prior to
contacting it, the nanowire diameter can be estimated. To estimate
this from the images, the convolution of nanowire and tip shape in
the STM image needs to be considered, especially if the tip has already
been used for contacting one or several other nanowires before. Figure 4d shows the resistance of the highly doped InP nanowires
plotted over their diameter with error bars indicating the estimated
uncertainty of the shape measurements. The clear decrease of the resistance R with increasing nanowire diameter d agrees
well with a classical resistance behavior of R ∼ 1/d2 (since confinement effects should
play only a minor role at the given diameters). Considering the measured
nanowire diameters and assuming a constant length of 2 μm, a
resistivity ρ = 13.3 (±5.3) Ω μm was obtained
for the individual nanowires. The resistivity is determined by the
charge carrier density n and their mobility μ
by ρ = (neμ)−1 with
the elementary charge e. If we assume a mobility
μ = 400 cm2 V–1 s–1, as was recently measured for similar H2S-doped InP nanowires,[41] the resistivity corresponds to a dopant concentration n = 1.2 × 1019 cm–3.One might ask whether the actual resistivity of the nanowires could
be even lower and if a part of the measured resistivity is due to
the contacts. We can exclude any significant resistance from the growth
substrate and its back contact, since the InP nanowires are grown
epitaxially on a highly n-doped InP (111)B wafer, resulting in a single-crystalline
interface. In order to evaluate the resistivity of the point contact
between the STMtip and the nanowire, we performed a first reference
measurement by establishing a point contact between the tip and the
nanowire growth substrate at various substrate positions, both between
nanowires and at areas of the substrate where no nanowires had been
grown, obtaining an average resistance of R = 0.49
(±0.21) kΩ. This value is a factor of 9 smaller than the
average nanowire resistance, although the surface of the growth substrate
consists of oxidized InP, while in the nanowire case the STMtip touches
an Au–In nanoparticle. Thus, the actual resistance of the tip–sample
point contact in the nanowire case is expected to be significantly
below 0.5 kΩ.In a further reference measurement, we evaporated
a ∼10
nm Au film onto a highly doped InAs substrate and annealed it in UHV
at 280 °C for 5 min, resulting in the formation of Au–In
islands with a diameter of about 100 nm, which is comparable to the
size of the metal nanoparticles on top of the nanowires. We imaged
these Au–In islands by STM and then established point contacts
between the STMtip and individual islands, thus simulating the situation
of the nanowire point contact measurements, only excluding the resistance
of the nanowires themselves. A very small average resistance of R = 21.6 (±1.4) Ω was obtained, which can be
regarded as the intrinsic resistance of our measurement setup, including
all series resistances of the STMtip and sample connections, the
sample back contact, and even the point contact between the STM probe
tip and a metal particle. Thus, the kΩ-range resistance measured
of individual nanowires can be attributed to the nanowire itself.Complementary to the highly doped InP nanowires, another nanowire
sample was investigated containing nonintentionally doped InAs nanowires
with diameters of about 100 nm. Resistance measurements on 10 individual
nanowires are shown in Figure 4b, all obtained
from linear I–V curves acquired with the STM
probe tip in point contact. The average resistance of these nanowires
is R = 4.3 (±2.3) × 105 Ω,
which is 100 times larger than for the highly doped InP nanowires.
This complementary data set demonstrates the generality of our method
to characterize nanowires of different materials and with orders of
magnitude difference in resistivity.It should be noted that
both material systems studied here, InAs
as well as highly doped InP, form Ohmic contacts with In–Au
alloys, of which the metal particles on top of the nanowires consist.
There are other nanowire systems like GaAs, which are known to form
Schottky barriers toward their Au-based metal particles, even though
those interfaces have shown much higher conductivity than comparable
bulk Schottky barriers.[28,46] Contacting the metal
particle of such nanowires by the STMtip can therefore not provide
direct resistance measurements of the nanowire itself but instead
investigate the I–V properties
of the highly interesting nanoscale interface. Indeed, with this method
it has been possible to measure the Schottky barrier height between
GaAs nanowires and their catalytic Au particles, as will be shown
elsewhere.[47]A unique advantage of
the present method is the well-controlled
formation of a point contact between the probe tip and the semiconductor
nanowire with very low resistance (less than 22 Ω). Compared
with other nanoprobe setups, the very clean environment of the STM
operated at UHV conditions without any electron beams, together with
STM probe tips being cleaned in vacuum and as-grown samples that are
free of processing-induced contamination, is highly beneficial for
the reproducible formation of Ohmic contacts to the nanowires.[36,48,49] The high resolution of the STM
in imaging semiconductor nanostructures[50−52] ensures that the tip-nanowire
point contact can be formed exactly at a specific position. Additionally,
the in situ sputtered STM tips, as shown in Figure 2b, exhibit a much smaller radius of curvature than typical
nanoprobes used elsewhere,[30,33] enabling very accurate
imaging of objects with as high aspect ratios as upright-standing
nanowires, as can be seen in Figure 1b. As
a result, our STM-based method provides a significantly more precise
positioning of the probe tip in respect to the center of the nanowire
than what can be achieved in SEM. This is even more remarkable since
our setup uses a single, standard STM, without the need for any complementary
microscopy techniques, which would make the entire method more delicate,
complicated, and expensive.Finally, we will discuss our method
in respect to conventional
resistivity measurements on individual nanowires in the FET geometry
using EBL-defined contacts. Although such measurements are well established,
they rely on approximations made for interpretation of the results,[26,27] and they imply elaborate sample preparation and processing steps,
which are not only time-consuming and expensive, but also expose the
nanowires to aggressive environments like strong electron beams and
chemical etching. Consequently, the reproducibility and quality of
EBL-defined nanowire contacts is still a major challenge: When a set
of individual nanowire devices is contacted, usually only a fraction
of them shows reasonable device characteristics, often enough the
formation of Ohmic contacts is not possible at all, as it was the
case in our reference experiment, Figure 4c,
while the majority of all our attempts to contact an individual nanowire
with the STMtip from top resulted in reproducible I–V curves with Ohmic contacts. Furthermore, studies with EBL-defined
contacts often show a large spread of the resistance measured for
individual nanowires,[22] often more than
an order of magnitude larger than with our method. For certain types
of more involved measurements and specific nanowires the I–V results can be improved in accuracy[25,53] and have also
been complemented by scanning gate microscopy data[54−56] or other scanning
probe studies.[57,58] However, even with the best EBL-defined
contacts the contact resistance still significantly influences the
measured resistance of the entire device.[23,24] In contrast, the STM-based method can be applied to as-grown nanowires
without any processing steps. Although STM in general is not a fast
technique, the time needed for preparing and measuring nanowire samples
until significant statistics on nanowire I–V properties are obtained is comparable in both approaches.In conclusion, we have successfully demonstrated how advanced device
characterization is possible on general nanowire samples using nothing
more than a standard STM. We image upright standing nanowires on-top,
enabling us to very accurately position the STMtip as nanoprobe,
and form a point contact with the nanowire. Ohmic contacts with an
extremely low contact resistance of less than 22 Ω could reproducibly
be established by this method for different nanowire material systems
and doping levels, already indicating the versatility of this method.
The very direct approach using as-grown nanowires without aggressive
or elaborate sample processing allows the characterization also of
very sensitive samples. On the other hand, it is possible to monitor
the I–V properties of individual nanowires
during various stages of device processing in a realistic upright
standing configuration. With the highly controllable conditions of
a UHV-based STM chamber, the new method is also well suited to investigate
how surface modifications like cleaning, oxidation, passivation, or
more advanced surface chemistry will change the transport properties
of individual nanowires. A first demonstration of comparing the I–V properties of more complex upright-standing
nanowires before and after chemical treatment is shown in Figure 1
of the Supporting Information. Furthermore,
the comparatively simple and compact setup using a conventional STM
without any further microscopy tools makes this method affordable,
flexible, and even suitable for transport measurements at extreme
conditions. Ultralow temperatures in the milliKelvin range, for example,
are nowadays accessible by STM,[59] but not
by SEM, TEM, or similar techniques. All these advantages make the
new method presented here to a unique tool for nondestructively measuring
resistivity and transport properties of a broad range of semiconductor
nanowires and nanowire devices with high reproducibility, accuracy,
and versatility.
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