Nov. 25, 2019

On the Advantages of High Vacuum Environments

How Vacuum Can Improve Conductive Atomic Force Microscopy

  • Fig. 1: 3D topography image overlaid with the current signal, recorded in high vacuum. Fig. 1: 3D topography image overlaid with the current signal, recorded in high vacuum.
  • Fig. 1: 3D topography image overlaid with the current signal, recorded in high vacuum.
  • Fig. 2: a)-c) Topography measurements on 1-2-layer sample, 3-4-layer sample and multilayer sample, d) schematic of sample structure of 3-4-layer sample and cAFM setup, e) height profile extracted at the position of the red line in b).
  • Fig. 3: Direct comparison of cAFM measurement in air and in high vacuum on a 3-4-layer sample. a) and b) topography, c) and d) current signal.
  • Fig. 4: cAFM measurement in high vacuum on 1-2-layer sample. a) sample topography and b) current signal.
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Insights into morphological and electronic properties of two-dimensional materials at the nanometer-scale are of great interest to the industry due to the decreasing sizes of semiconductor devices. Complementary atomic force microscopy (AFM) techniques like conductive AFM allow simultaneous insights into electronic and structural sample information. Conductive AFM in high vacuum offers an additional improvement in the sensitivity of the electronic measurement signals due to the removal of the surface water layer.
Since the discovery of graphene in 2004 [1], two-dimensional (2D) materials have seen a growing interest in the scientific community. Researchers have synthesized and characterized a variety of 2D materials, including the group of transition metal dichalcogenides (TMDs) [2-6]. TMDs attracted the attention of the semiconductor industry, because many of the compounds are direct band gap semiconductors with low dielectric constants and high charge-carrier mobilities. Due to their layer thickness of less than 1 nm, TMDs qualify as promising candidates for semiconductor devices below 5 nm following the trend of ever lower device sizes according to Moore’s law. However, the integration of TMDs in commercial semiconductor devices still faces some challenges. As such, the desired electronic properties often are limited to individual islands or grains and controlled layer growth, transfer and processing of high-quality TMD films remain complicated [7-9].
Electrical atomic force microscopy (AFM) is ideally suited to visualize local differences in the electronic properties of TMD films with a nanometer-resolution. In AFM, a nanometer-sized tip at the end of a cantilever scans sample surfaces. From the deflection of the cantilever at each point of the sample, the surface structure is then reconstructed and assembled into a topography image. Using a conductive cantilever/tip-system and establishing a mechanical contact between tip and sample facilitates conductive AFM (cAFM) measurements with an applied bias. cAFM allows resolving the spatial distribution of heterogeneous conductivities in addition to the sample topography.

For this purpose, cAFM records the current flow between the cantilever/tip-system and the sample at varying sample biases with the aid of a current-voltage preamplifier. Since cAFM is a contact mode AFM method, the use of soft cantilevers with low spring constants is advantageous to minimize tip wear or sample damage.

This article compares cAFM measurements on the TMD-material molybdenum disulfide (MoS2) in air and in a high vacuum environment of less than 1 ∙ 10-5 Torr achieved by the Park NX-Hivac AFM (fig. 1). Generally, a thin layer of water forms on surfaces in ambient conditions, which can reduce the quality and sensitivity of the conductivity measurement in cAFM. Additionally, water induces a p-doping in MoS2, therefore limiting the electrical conductivity of the material.
Atomic Force Microscopy on MoS2
Figure 2 summarizes topography measurements on three MoS2 samples with different layer thicknesses: one sample with 1-2 MoS2 layers (a), one sample with 3-4 MoS2 layers (b), and another multi-layer sample with pyramidal surface structures (c). The 1-2-layer sample consists of one closed MoS2 monolayer with additional single-layered islands, featuring a step height of 0.6 nm - the layer thickness of a single monolayer. The islands represent the onset of the growth of the second layer and can be recognized in figure 2 as bright regions in the topography. Similarly, the 3-4-layer sample comprises a closed three-layered MoS2 film with additional single-layer islands. Figure 2d schematically shows the basic structure of the 3-4-layer sample as well as the cAFM experimental setup for the following measurements. Here, each green layer represents one MoS2 monolayer, while the grey arrangement on the left side is the electrical contact required to apply of the sample bias during the cAFM measurement. The multi-layered MoS2 sample differs strongly from the former in its surface structure. This sample exhibits three-dimensional (3D) pyramid-shaped features on top of a closed 3-layer MoS2 film. The formation of the pyramid-shaped features originates from a change of the growth mechanism from layer-by-layer to a 3D growth at thicknesses beyond 4 layers [10].
In addition to the MoS2 islands, the AFM imaged steps in the topography of the 1-2-layer and 3-4-layer samples that run diagonally across both images in figure 2a and b. These lines originate from the terrace structure of the underlying sapphire substrate, which the AFM detected through the MoS2 films. However, the height of the steps allows a clear distinction between sapphire terraces and MoS2 steps: While the characteristic step height on the c-plane of the sapphire substrate is 0.2 nm, a monolayer MoS2 has a thickness of 0.6 nm. The height profile in figure 2e visualized the different step heights of the substrate and the MoS2 sample [11,12].
Conductivity in Air and High Vacuum
In order to demonstrate the advantageous effects of high vacuum on the quality of cAFM, comparative measurements in air and in vacuum <1∙10-5 Torr were carried out on the same sample. While the topography images in air and high vacuum appeared largely similar (fig. 3a and b), cAFM data differed significantly (fig. 3c and d). Here, the average current increased by three orders of magnitude in high vacuum compared to the measurement in air. In air, the average current was 1.4 nA at 5 V sample bias. In high vacuum on the other hand the average current increased to 1.1 μA with the same sample bias. The increase in average current originates from the removal of the thin layer of water that forms on the surface of materials in air due to the humidity level in ambient conditions. This layer of water is particularly problematic for MoS2 because water p-dopes the material and therefore becomes insulating. The cAFM results agree with the results of previous studies, in which researchers showed that the on-state current and charge-carrier mobility in MoS2 semiconductor devices dropped significantly after contact with deionized water [13].
In addition to the overall increase in the average current, cAFM improved in sensitivity for the measurements in a high vacuum environment. While the current image recorded in air appeared largely homogeneous without defined features, cAFM in high vacuum was able to detect fine structures in the current channel. As such, cAFM revealed that the current at grain boundaries and step edges of the MoS2 islands decreases. Figure 4 shows the reduced current flow at step edges on a 1-2-layer sample that could not be resolved in air (fig. 3c). The decrease in the detected current at the position of step edges and grain boundaries translates into a local reduction in conductivity. Thus, these topographic features act as electrostatic barriers on the charge-carrier transport and are detrimental for the implementation of MoS2 in commercial semiconductor devices. This correlative current-topo­graphy behavior may have been missed if not for the increased sensitivity of cAFM in high vacuum.
This study examined the morphological and electrical properties of the 2D material MoS2. The direct comparison of cAFM measurements in air and in a vacuum <1∙10-5 Torr demonstrated that the water layer on the sample surface in air considerably lowered the reliability of cAFM. Removal of this water layer in high vacuum increased the current by three orders of magnitude. Furthermore, cAFM in high vacuum allowed imaging of finer structures, thus enabling researchers to resolve the reduced current flow at the MoS2 step edges.
Jonathan Ludwig1,2, Marco Mascaro1,2, Umberto Celano1, Ilka M. Hermes3, Wilfried Vandervorst1,2, Kristof Paredis1
1IMEC, Leuven, Belgium
2Department of Physics and Astronomy, University of Leuven, Leuven, Belgium
3Park Systems Europe GmbH, Mannheim, Germany
Ilka M. Hermes
Park Sytems Europe GmbH


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