Variable-temperature independently driven four-tip scanning tunneling microscope

The authors have developed an ultrahigh vacuum (UHV) variable-temperature four-tip scanning tunneling microscope (STM), operating from room temperature down to 7 K, combined with a scanning electron microscope (SEM). Four STM tips are mechanically and electrically independent and capable of positioning in arbitrary configurations in nanometer precision. An integrated controller system for both of the multitip STM and SEM with a single computer has also been developed, which enables the four tips to operate either for STM imaging independently and for four-point probe (4PP) conductivity measurements cooperatively. Atomic-resolution STM images of graphite were obtained simultaneously by the four tips. Conductivity measurements by 4PP method were also performed at various temperatures with the four tips in square arrangement with direct contact to the sample surface.     

Iterative image-based modeling and control for higher scanning probe microscope performance

In this article, we develop an image-based approach to model and control the dynamics of scanning probe microscopes (SPMs) during high-speed operations. SPMs are key enabling tools in the experimental investigation and manipulation of nano- and subnanoscale phenomena; however, the speed at which the SPM probe can be positioned over the sample surface is limited due to adverse dynamic effects. It is noted that SPM speed can be increased using model-based control techniques. Modeling the SPM dynamics is, however, challenging because currently available sensing methods do not measure the SPM tip directly. Additionally, the resolution of currently available sensing methods is limited by noise at higher bandwidth. Our main contribution is an iterative image-based modeling method which overcomes these modeling difficulties (caused by sensing limitations). The method is applied to model an experimental scanning tunneling microscope (STM) system and to achieve high-speed imaging. Specifically, we model the STM up to a frequency of 2000 Hz (corresponds to approximately 23 of the resonance frequency of our system) and achieve approximately 1.2% error in 1 nm square images at that same frequency.     

A cryogenic Quadraprobe scanning tunneling microscope system with fabrication capability for nanotransport research

We describe the development and the capabilities of an advanced system for nanoscale electrical transport studies. This system consists of a low temperature four-probe scanning tunneling microscope (STM) and a high-resolution scanning electron microscope coupled to a molecular-beam epitaxy sample preparation chamber. The four STM probes can be manipulated independently with subnanometer precision, enabling atomic resolution STM imaging and four-point electrical transport study of surface electronic systems and nanostructured materials at temperatures down to 10 K. Additionally, an integrated energy analyzer allows for scanning Auger microscopy to probe chemical species of nanostructures. Some testing results are presented.     

A data acquisition and image processing system for scanning tunneling microscopy

We have built a dedicated data acquisition and image processing system for scanning tunneling microscopy (STM). Data acquisition is accomplished by a fast 8-bit add-on frame grabber which may be synchronized either to standard TV frequencies or to asynchronous slow scan data sources such as STM or SEM. A 32-bit minicomputer is used for image processing by means of a comprehensive interactive-language which also allows the data acquisition process to be controlled. To speed up time-consuming computations, a floating-point array processor was linked to the system.     

STM/SEM correlative study of facetted gold

We have integrated an STM unit with a conventional scanning electron microscope in order to perform STM–SEM correlative microscopy. The method is applied to an electrochemically facetted gold sample, which provides a surface structure suitable for this study. We discuss the factors which are relevant in order to obtain a quantitative resolution of the topographic surface structure, by taking advantage of the performances of both techniques. In particular we suggest the use of the STM height distribution as the best parameter for STM/SEM correlation. Finally, from the STM data we deduce that the main process during electrochemical etching is the formation of (111) faces.     

A nanopositioner for scanning probe microscopy: the KoalaDrive

We present a new type of piezoelectric nanopositioner called KoalaDrive which can have a diameter less than 2.5 mm and a length smaller than 10 mm. The new operating principle provides a smooth travel sequence and avoids shaking which is intrinsic to nanopositioners based on inertial motion with sawtooth driving signals. In scanning probe microscopy, the KoalaDrive can be used for the coarse approach of the tip or sensor towards the sample. Inserting the KoalaDrive in a piezo tube for xyz-scanning integrates a complete scanning tunneling microscope (STM) inside a 4 mm outer diameter piezo tube of <10 mm length. The use of the KoalaDrive makes the scanning probe microscopy design ultracompact and accordingly leads to a high mechanical stability. The drive is UHV, low temperature, and magnetic field compatible. The compactness of the KoalaDrive allows building a multi-tip STM as small as a single tip STM.     

Developments of scanning probe microscopy with stress/strain fields

An innovative stress/strain fields scanning probe microscopy in ultra high vacuum (UHV) environments is developed for the first time. This system includes scanning tunneling microscope (STM) and noncontact atomic force microscope (NC-AFM). Two piezo-resistive AFM cantilever probes and STM probes used in this system can move freely in XYZ directions. The nonoptical frequency shift detection of the AFM probe makes the system compact enough to be set in the UHV chambers. The samples can be bent by an anvil driven by a step motor to induce stress and strain on their surface. With a direct current (dc) power source, the sample can be observed at room and high temperatures. A long focus microscope and a monitor are used to observe the samples and the operation of STM and AFM. Silicon(111) surface in room temperature and silicon(001) surface in high temperature with stress were investigated to check the performance of the scanning probe microscope.     

Antenna-based ultrahigh vacuum microwave frequency scanning tunneling microscopy system

The instrumental synthesis of high resolution scanning tunneling microscopy (STM) with the ability to measure differential capacitance with atomic scale resolution is highly desirable for fundamental metrology and for the study of novel physical characteristics. Microwave frequency radiation directed at the tip-sample junction in an STM system allows for such high-resolution differential capacitance information. This ability is particularly critical in ultrahigh vacuum environments, where the additional parameter space afforded by including a capacitance measurement would prove powerful. Here we describe the modifications made to a commercial scanning tunneling microscope to allow for broad microwave frequency alternating current scanning tunneling microscopy (ACSTM) in ultrahigh vacuum conditions using a relatively simple loop antenna and microwave difference frequency detection. The advantages of our system are twofold. First, the use of a removable antenna on a commercial STM prevents interference with other UHV processes while providing a simple method to retrofit any commercial UHV-STM with UHV-ACSTM capability. Second, mounting the microwave antenna on a translator allows for specific tuning of the system to replicate experimental conditions between samples, which is particularly critical in sensitive systems like organic thin films or single molecules where small changes in incident power can affect the results. Our innovation therefore provides a valuable approach to give nearly any commercial STM, be it an ambient or UHV system, the capability to measure atomic-scale microwave studies such as differential capacitance or even single molecule microwave response, and it ensures that experimental ACSTM conditions can be held constant between different samples.     

MEMS-based fast scanning probe microscopes

Scanning probe microscopy is a frequently used nanometer-scale surface investigation technique. Unfortunately, its applicability is limited by the relatively low image acquisition speed, typically seconds to minutes per image. Higher imaging speeds are desirable for rapid inspection of samples and for the study of a range of dynamic surface processes, such as catalysis and crystal growth. We have designed a new high-speed scanning probe microscope (SPM) based on micro-electro mechanical systems (MEMS). MEMS are small, typically micrometer size devices that can be designed to perform the scanning motion required in an SPM system. These devices can be optimized to have high resonance frequencies (up to the MHz range) and have very low mass (10⁻¹¹ kg). Therefore, MEMS can perform fast scanning motion without exciting resonances in the mechanical loop of the SPM, and hence scan the surface without causing the image distortion from which conventional piezo scanners suffer. We have designed a MEMS z-scanner which we have integrated in commercial AFM (atomic force microscope) and STM (scanning tunneling microscope) setups. We show the first successful AFM experiments.     

Large-area profile measurement of sinusoidal freeform surfaces using a new prototype scanning tunneling microscopy

This paper presents large-area profile measurement of ultra-precision diamond turned sinusoidal surfaces by using a specially developed scanning tunneling microscopy (STM). The new prototype of STM system employs a long stroke PZT servo actuator as the Z-directional scanner, an integrated capacitance displacement sensor to accurately measure the Z-directional profile height, a motorized stage with long traveling stroke for carrying out large-area scanning. A simple method for self-calibration of the inevitable sample tilt is proposed in order to achieve large-area measurement without tip-crashing or losing of tip-sample interaction. Several types of ultra-precision machined sinusoidal freeform surfaces with different geometrical parameters are measured by the new STM system over large scanning areas at the scale of millimeters. Specially, a sinusoidal surface with peak-valley amplitude of 22 μm and periodical wavelength of 550 μm is successfully measured and imaged by the STM system. The measurement repeatability error, repeatability standard deviation and measured profile deviation are also evaluated. It is confirmed that the new STM system is capable of carrying out large-area as well as large-amplitude measurement of the ultra-precision machined sinusoidal surfaces.     

Surface investigations with a combined scanning electron–scanning tunneling microscope

We have combined a scanning tunneling microscope (STM) with a scanning electron microscope (SEM) for surface investigations of atomically flat surfaces, ultrathin adsorbate films, and material surfaces. The mechanical stability of the hybrid instrument allows high-resolution SEM of samples mounted on the STM stage and atomic resolution with the STM. Experimental results of combined SEM/STM investigations on textured material surfaces, submicron structures, and atomically flat conducting surfaces are presented. An example is given for surface machining with the STM under SEM control.     

Combined low-temperature scanning tunneling/atomic force microscope for atomic resolution imaging and site-specific force spectroscopy

We present the design and first results of a low-temperature, ultrahigh vacuum scanning probe microscope enabling atomic resolution imaging in both scanning tunneling microscopy (STM) and noncontact atomic force microscopy (NC-AFM) modes. A tuning-fork-based sensor provides flexibility in selecting probe tip materials, which can be either metallic or nonmetallic. When choosing a conducting tip and sample, simultaneous STM/NC-AFM data acquisition is possible. Noticeable characteristics that distinguish this setup from similar systems providing simultaneous STM/NC-AFM capabilities are its combination of relative compactness (on-top bath cryostat needs no pit), in situ exchange of tip and sample at low temperatures, short turnaround times, modest helium consumption, and unrestricted access from dedicated flanges. The latter permits not only the optical surveillance of the tip during approach but also the direct deposition of molecules or atoms on either tip or sample while they remain cold. Atomic corrugations as low as 1 pm could successfully be resolved. In addition, lateral drifts rates of below 15 pm/h allow long-term data acquisition series and the recording of site-specific spectroscopy maps. Results obtained on Cu(111) and graphite illustrate the microscope's performance.     

Nanomanipulation and nanofabrication with multi-probe scanning tunneling microscope: from individual atoms to nanowires

The wide variety of nanoscale structures and devices demands novel tools for handling, assembly, and fabrication at nanoscopic positioning precision. The manipulation tools should allow for in situ characterization and testing of fundamental building blocks, such as nanotubes and nanowires, as they are built into functional devices. In this paper, a bottom-up technique for nanomanipulation and nanofabrication is reported by using a 4-probe scanning tunneling microscope (STM) combined with a scanning electron microscope (SEM). The applications of this technique are demonstrated in a variety of nanosystems, from manipulating individual atoms to bending, cutting, breaking carbon nanofibers, and constructing nanodevices for electrical characterizations. The combination of the wide field of view of SEM, the atomic position resolution of STM, and the flexibility of multiple scanning probes is expected to be a valuable tool for rapid prototyping in the nanoscience and nanotechnology.     

Imaging biological macromolecules by STM: quantitative interpretation of topographs

Methods are discussed which permit the calibration of x-, y-, z-sensitivities, non-linearities and frequency responses of the scanning device of a scanning tunneling microscope (STM) either by interferometry or directly from STM topographs. A technique is presented to measure the frequency response of the complete STM feedback unit and to derive a maximum speed in z direction which allows one to estimate the maximum scanning speed still permitting one to track surface corrugations. The signal transfer characteristics of a STM are evaluated in a direct comparison with high resolution transmission electron microscopy on an identical specimen area. The various effects of contaminants between tip and specimen and the finite tip radius receive special attention.     

The FAST module: an add-on unit for driving commercial scanning probe microscopes at video rate and beyond

We present the design and the performance of the FAST (Fast Acquisition of SPM Timeseries) module, an add-on instrument that can drive commercial scanning probe microscopes (SPM) at and beyond video rate image frequencies. In the design of this module, we adopted and integrated several technical solutions previously proposed by different groups in order to overcome the problems encountered when driving SPMs at high scanning frequencies. The fast probe motion control and signal acquisition are implemented in a way that is totally transparent to the existing control electronics, allowing the user to switch immediately and seamlessly to the fast scanning mode when imaging in the conventional slow mode. The unit provides a completely non-invasive, fast scanning upgrade to common SPM instruments that are not specifically designed for high speed scanning. To test its performance, we used this module to drive a commercial scanning tunneling microscope (STM) system in a quasi-constant height mode to frame rates of 100 Hz and above, demonstrating extremely stable and high resolution imaging capabilities. The module is extremely versatile and its application is not limited to STM setups but can, in principle, be generalized to any scanning probe instrument.     

Rapid measurement of a high step microstructure with 90° steep sidewall

A prototype STM system with high aspect ratio measurement capability is developed to fulfill accurate profile measurement of a high step microstructure with 90° steep sidewall. Distinguished from the traditional STM, the new system consists of a long range piezoelectric (PZT) actuator with full stroke of 60 μm as Z-direction servo scanner, a specially customized high aspect ratio STM probe with effective tip length of 300 μm, and an X-Y motorized driven stage for planar scanning. A tilt stage is used to adjust the probe-sample relative angle to compensate the evitable non-parallel effects. Based on the new STM system, sample-tilt-scanning methodology is proposed for eliminating the scanning blind region between the probe and the microstructure. A high step microstructure with height of 23 μm, 90° steep sidewall and width of 50μm has been successfully measured. The slope angle of the sidewall has been achieved to be 85° and the step height at the rising edge and the trench depth at the falling edge are both measured to be 22.96 μm. The whole measuring process only spent less than 10 min. It provides an effective and nondestructive solution for the measurement of high step or deep trench microstructures. In addition, this work also opens the way for further study on sidewall roughness and the tip-sample interaction at the edge of the sidewall, which are highly valuable for fabrication and quality control of high step microstructures.     

Light emission induced by tunneling electrons from surface nanostructures observed by novel conductive and transparent probes

We have developed an ultrahigh-vacuum low-temperature scanning tunneling microscope (STM) equipped with a near-field optical detection system using novel conductive and optically transparent probes. Tunneling-electron induced photons generated in a nanometer-scale area just under the STM probe can be collected directly into the core of the optical fiber probe within the optical near-field region. Firstly, optical fiber probes coated with indium-tin-oxide thin film are applied to quantitative analysis of p-type GaAs(110) surface, where a decrease of light emission in photon mapping clearly extracts the existence of Zn accepter atoms located at the sub-surface layers. Secondly, in order to enhance the efficiency for inelastic tunneling excitation of a tip-induced plasmon mode, a STM probe coated with an Ag/ITO dual-layer film has been developed and applied to an Ag(111) surface, where photon mapping with a step resolution has been achieved by near-field detection.     

Vertical inertial sliding drive for coarse and fine approaches in scanning probe microscopy

Mechanisms for controlled approach of a probe tip toward the sample surface are essential in high resolution imaging by scanning probe microscopy (SPM). This work describes the development and performance of an inertial sliding drive capable of translating a relatively large mass (25 g) at up to 1 mms over 1 cm with step sizes of 10-250 nm in ambient conditions using various wave forms as measured by fiber optic interferometry. The drive functions independent of orientation with a threshold voltage of less than 15 V using a single drive signal. Use of piezotube actuators in a radially symmetric arrangement provides guided motion and minimizes differential thermal expansion between critical components. Controlled translation of the entire scanning component in both ambient and electrochemical scanning tunneling microscopy has been routinely achieved with no evidence of tip crash. This device has been specifically designed for use in in situ SPM applications where stability of the sample and that of the liquid environment are paramount.     

Scanning tunneling microscope combined with scanning electron microscope

A scanning tunneling microscope (STM) has been installed in a usual scanning electron microscope (SEM) with a vacuum of 10⁻⁶ Torr. The STM image is displayed on the cathode ray tube of the SEM, 512 × 512 pixels, with a scanning rate of 80 s/picture. The spatial resolution of the STM is about 1 Å, while that of the SEM is several tens of ångströms. The combined scanning microscope covers a wide magnification range from 10 to 10⁷, where STM covers the high magnification region from 10⁵ to 10⁷.     

Atom probe,AFM, and STM studies on vacuum-fired stainless steels

The surface morphology of grades 304L and 316LN stainless steels, after low-temperature bake-out process and vacuum annealing, has been studied by atomic force microscopy (AFM) and scanning tunnelling microscopy (STM). The local elemental composition on the surface before and after thermal treatment has been investigated by atom probe (AP) depth profiling measurements. After vacuum annealing, AFM and STM show significant changes in the surface structure and topology. Recrystallization and surface reconstruction is less pronounced on the 316LN stainless steel. AP depth profiling analyses result in noticeable nickel enrichment on the surface of grade 304L samples. Since hydrogen recombination is almost controlled by surface structure and composition, a strong influence on the outgassing behaviour by the particular surface microstructure can be deduced.