L. Tröger

Concept for support and cleavage of brittle crystals

We report on sample holders for crystals to be cleaved for the preparation of surfaces with large atomically flat terraces. The concept for mounting sample crystals is based on a vicelike clamping mechanism to securely hold the crystal in position while reducing the risk of fragmentation. Sample holders based on this concept and made of suitable materials allow preparation and cleavage of crystals in the ultrahigh vacuum at high or low temperatures. To cleave the crystal, we employ a scalpel blade mounted on a wobble stick to generate a highly localized stress field initiating the cleavage process. The sample holders are used for experiments of highest resolution scanning force microscopy, however, the concept can be transferred to any other system where cleavage faces of crystals are of interest. Exemplarily, scanning force microscopy results demonstrate that (111) cleavage faces of CaF2 crystals can be prepared with steps only a few F-Ca-F triple-layers high and atomically flat terraces extending over areas of several microm2.

Achieving high effective Q-factors in ultra-high vacuum dynamic force microscopy

The effective Q-factor of the cantilever is one of the most important figures-of-merit for a non-contact atomic force microscope (NC-AFM) operated in ultra-high vacuum (UHV). We provide a comprehensive discussion of all effects influencing the Q-factor and compare measured Q-factors to results from simulations based on the dimensions of the cantilevers. We introduce a methodology to investigate in detail how the effective Q-factor depends on the fixation technique of the cantilever. Fixation loss is identified as a most important contribution in addition to the hitherto discussed effects and we describe a strategy for avoiding fixation loss and obtaining high effective Q-factors in the force microscope. We demonstrate for room temperature operation, that an optimum fixation yields an effective Q-factor for the NC-AFM measurement in UHV that is equal to the intrinsic value of the cantilever.

Improvement of a dynamic scanning force microscope for highest resolution imaging in ultrahigh vacuum

We report on a modification of a commercial scanning force microscope (Omicron UHV AFM/STM) operated in noncontact mode (NC-AFM) at room temperature in ultrahigh vacuum yielding a decrease in the spectral noise density from 2757 to 272 fm/Hz. The major part of the noise reduction is achieved by an exchange of the originally installed light emitting diode by a laser diode placed outside the vacuum, where the light is coupled into the ultrahigh vacuum chamber via an optical fiber. The setup is further improved by the use of preamplifiers having a bandpass characteristics tailored to the cantilever resonance frequency. The enhanced signal to noise ratio is demonstrated by a comparison of atomic resolution images on CeO(2)(111) obtained before and after the modification.

Clear Signature of the (2 × 1) Reconstruction of Calcite (101̅4)

Calcite is a mineral of fundamental importance that plays a crucial role in many fields of research such as biomineralization, biomolecule adsorption, and reactivity as well as industrial and daily life applications. Consequently, the most stable cleavage plane of calcite has been studied extensively using both direct imaging techniques such as atomic force microscopy as well as spectroscopic and diffraction techniques. Several surface structures have been reported for the (1014) cleavage plane of calcite differing from the simple bulk-truncated structure and an ongoing controversy exists in literature whether the cleavage plane exhibits a (2 x 1) reconstruction or not. We study the (1014) cleavage plane using high-resolution noncontact atomic force microscopy (NC-AFM) under ultrahigh vacuum conditions and obtain a clear signature of the (2 x 1) reconstruction. This reconstruction is observed in very narrow tip-surface distance ranges only, explaining why in some experiments the reconstruction has been observed and in others not. Moreover, as all sample preparation is performed in ultrahigh vacuum, the possibility of the (2 x 1) reconstruction being adsorbate-induced appears rather unlikely. Additionally, tip-induced surface changes are ruled out as origin for the observed reconstruction either. In conclusion, our study suggests that the (2 x 1) reconstruction is a true surface property of the (1014) cleavage plane of calcite.

Modification of a commercial atomic force microscopy for low-noise, high-resolution frequency-modulation imaging in liquid environment

A key issue for high-resolution frequency-modulation atomic force microscopy imaging in liquids is minimizing the frequency noise, which requires a detailed analysis of the corresponding noise contributions. In this paper, we present a detailed description for modifying a commercial atomic force microscope (Bruker MultiMode V with Nanoscope V controller), aiming at atomic-resolution frequency-modulation imaging in ambient and in liquid environment. Care was taken to maintain the AFMs original stability and ease of operation. The new system builds upon an optimized light source, a new photodiode and an entirely new amplifier. Moreover, we introduce a home-built liquid cell and sample holder as well as a temperature-stabilized isolation chamber dedicated to low-noise imaging in liquids. The success of these modifications is measured by the reduction in the deflection sensor noise density from initially 100 fm/√Hz to around 10 fm/√Hz after modification. The performance of our instrument is demonstrated by atomically resolved images of calcite taken under liquid conditions.

Carbon tips as sensitive detectors for nanoscale surface and sub-surface charge

Electrically insulating tips prepared by carbon deposition are used as sensitive detectors of nanoscale charge patterns on cleaved insulating surfaces. Dynamic scanning force microscopy images recorded with a neutral carbon tip reveal the surface topography and strong local charging at step edges while images taken with a charged tip exhibit subtle contrast features resulting from charges located at or beneath the surface of flat terraces. Analysing dynamic phenomena during imaging allows a determination of charge polarity and identifies sub-surface charges as trapping centres for charges exchanged between the tip and the surface. A density of a few hundred charged sub-surface defects per μm2 is determined on while the defect density is one order of magnitude smaller on CaF2(111). The method allows the detection of elementary charges at room temperature.

Versatile system for the temperature-controlled preparation of oxide crystal surfaces

We present a versatile system for the preparation of oxide crystal surfaces in the ultra-high vacuum (UHV) at temperatures up to 1300 K. Thermal treatment is accomplished by direct current heating of a tantalum foil in contact with the oxide sample. The sample temperature is measured by a thermocouple at a position close to the crystal and its reading is calibrated against the surface temperature determined by a second thermocouple temporarily attached to the surface. The design of the sample holder is based on a transferable plate originally developed for a commercial UHV scanning probe microscope. The system is, however, also suitable for the use with electron spectroscopy or electron diffraction based surface analytical techniques. We present results for the high-temperature preparation of CeO(2)(111) surfaces with atomically flat terraces exhibiting perfect atomic order and cleanliness as revealed by non-contact atomic force microscopy (NC-AFM) imaging. NC-AFM imaging is, furthermore, used to demonstrate the temperature-controlled aggregation of gold atoms on the CeO(2)(111) surface and their evaporation at high temperatures.

Quantification of antagonistic optomechanical forces in an interferometric detection system for dynamic force microscopy

In fiber-optic interferometer systems detecting oscillatory cantilever motion, the intensity distribution of the light field in the interferometric cavity generates an optomechanical coupling determining the effective properties of the oscillating system. For a low finesse cavity established by an uncoated cantilever and the fiber end, the resonance frequency and spring constant are shifted mainly due to radiation pressure whereas the Q-factor is varied due to photothermal forces under typical conditions. We find, that radiation pressure and photothermal force act in opposite directions and discuss the retardation times governing the antagonistic effects differing by orders of magnitude.

Atomic resolution force microscopy imaging on a strongly ionic surface with differently functionalized tips

Three types of tips for noncontact atomic force microscopy imaging, namely, a silicon nanopillar tip, a carbon nanopillar tip, and a fluoride cluster tip, are prepared for atomic resolution imaging on the CaF2(111) surface. The most enhanced atomic corrugation is obtained with the fluoride cluster tip prepared by gently touching the fluorite surface. Atom resolved images are much harder to obtain with the other tips. This demonstrates the importance of having a polar tip for atomic resolution imaging of an ionic surface and supports the general notion that a surface is best imaged with a tip of the same material.

Concept for support and heating of plate-like samples in the ultra-high vacuum.

We present the concept for a sample holder designed for mounting and heating of plate-like samples that is based on a clamping mechanism for easy handling. The clamping mechanism consists of a U-shaped bracket encompassing the sample support plate from the rear. Two spring wires are fixed in the walls of the bracket spanning the sample to secure it with only two point contacts. This enables the sample to freely expand or contract during heating and cooling. To accommodate for a large variety in sample size, shape, and quality, we introduce two designs differing in the generation of the clamping force: One pressing the sample against the spring wires, the other one pulling the spring wires onto the sample. Both designs yield an automatically even alignment of the sample during the mounting process to achieve an even load distribution and reliable fixation specifically for brittle samples. For high temperature treatment, the sample holders are enhanced by a resistive heating plate. As only the sample and a small fraction of the sample holder are heated, temperatures of 1300 °C are reached with only 8 W heating power. The sample support and heating components are mounted on a 11 mm × 13 mm base plate with a handle that can be transferred between the sample entry stage, the preparation stage, and surface science experiments in the ultra-high vacuum system.