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.     

18/20 T high magnetic field scanning tunneling microscope with fully low voltage operability, high current resolution, and large scale searching ability

We present a home-built 18/20 T high magnetic field scanning tunneling microscope (STM) featuring fully low voltage (lower than ±15 V) operability in low temperatures, large scale searching ability, and 20 fA high current resolution (measured by using a 100 GOhm dummy resistor to replace the tip-sample junction) with a bandwidth of 3.03 kHz. To accomplish low voltage operation which is important in achieving high precision, low noise, and low interference with the strong magnetic field, the coarse approach is implemented with an inertial slider driven by the lateral bending of a piezoelectric scanner tube (PST) whose inner electrode is axially split into two for enhanced bending per volt. The PST can also drive the same sliding piece to inertial slide in the other bending direction (along the sample surface) of the PST, which realizes the large area searching ability. The STM head is housed in a three segment tubular chamber, which is detachable near the STM head for the convenience of sample and tip changes. Atomic resolution images of a graphite sample taken under 17.6 T and 18.0001 T are presented to show its performance.     

Electrical detection of β-amyloid (1-40) using scanning tunneling microscopy

Numerous studies have shown that the presence of β-amyloid (1-40) in cerebrospinal fluid can be used as a potential biomarker for Alzheimer's disease. Identifying biomarkers for Alzheimer's disease is highly important because these biomarkers could be used to establish the diagnosis before the disease reaches clinical severity. In this study, a vertically configured electrical detection system associated with scanning tunneling microscopy (STM) was used to characterize antigen–antibody binding interactions. The proposed technique can be easily utilized to construct a multiple measurement system in a protein chip. The immunocomplexes used in the model protein comprise β-amyloid (1-40), corresponding antibody fragments, and gold nanoparticle–antibody conjugates. The electrical tunneling current between the STM tip and these complexes exhibited a peak-like pulse, where the frequency of these pulses was dependent on the surface density of bound complexes. Hence, a quantitative measurement of β-amyloid concentration from a periodogram analysis of peak frequency was successfully achieved at concentrations as low as 1 fg/mL.     

Differential scanning tunnelling microscopy

We review the principle of differential imaging and its application to scanning tunnelling microscopy (STM). It is shown that placing a lateral dither on an STM tip at high frequency provides the means for transfering topographic information to a frequency range where noise is small. Differential STM imaging on graphite and gold is demonstrated. A simple relation between the differential image and the conventional topographic image is described.     

A fully automated, ‘thimble-size’ scanning tunnelling microscope

A novel, fully automated high-stability, high-eigenfrequency scanning tunnelling microscope (STM) has been developed. Its key design feature is the application of two piezoelectric ceramic tubes, one for the x-y-z motion of the tip and one for a linear motor (‘nano-worm’) used for the coarse positioning of the tip relative to the specimen. By means of the nano-worm, the tip can be advanced in steps between 16 and 0·2 nm. The walking distance is >2 mm, with a maximum speed of 2000 steps/s. The nano-worm positioning implies that this STM is fully controlled by electronic means, and that no mechanical coupling is needed, which makes operation of the STM extremely convenient. The axial-symmetry construction is rigid, small and temperature-compensated, yielding reduced sensitivity to mechanical and acoustic vibrations and temperature variations. The sample is simply placed on a piece of invar which surrounds the scanner tube and the nano-worm and is held by gravity alone. This allows for easy sample mounting. The performance of the microscope has been tested in air by imaging a variety of surfaces, including graphite and biological samples.     

Electrically conductive and optically transparent Sb-doped SnO2 STM-probe for local excitation of electroluminescence

We demonstrate that an optically transparent and electrically conductive antimon-doped tin-oxide tip that is prepared in a sol-gel process can be used as a probe for scanning tunnelling microscopy (STM), yielding atomic vertical and nanometre lateral resolution. Emission of visible light from the tunnelling junction between gold particles and the tip is observed for bias voltages above 7 V. In contrast to the metallic tips generally used in STM, this tip does not significantly perturb the local optical response. Therefore, the tunnelling induced light can be used to map the optical near-field of surface structures with the tunnel gap acting as highly localised light source for the investigation of near-field enhancement in complex metal structures.     

High-resolution scanning tunneling microscopy for molecules

Scanning tunneling microscopy (STM) can detect individual molecular configuration with its high spatial resolution ability, but some intrinsical and extrinsic factors result in the complexities of STM imaging of single molecules. By combining STM experimental work and theoretical simulation with the local density approximation based on Bardeen perturbation method, we have explored the atomic-scale configuration of the following molecular systems: C(60) molecules adsorbed on Si(111)-(7x7); alkanethiol self-assembly monolayers on Au(111); C(60) molecule imaged by STM tip adsorbed with another C(60) molecule; O(2) molecule adsorbed on Ag(110) and CO molecule adsorbed on Cu(111) imaged by CO chemically modified STM tip. Some related problems including: molecule-substrate interactions, STM imaging mechanism, chemically modified STM tip, etc., are discussed.     

Donor graphite intercalation compounds studied with a high stability STM

We have designed a small, rigid and easy operable scanning tunnelling microscope (STM) which shows low thermal drift rates due to its compact construction and the chosen materials. Using this instrument we have studied stage 1 donor graphite intercalation compounds (C₆Li and C₈K) with atomic resolution either in the current imaging, constant current or local tunnelling barrier height mode of operation. Ordered superlattices commensurate as well as incommensurate with the graphite lattice have been observed on the C₆Li surface. STM images on C₈K revealed a graphitic surface structure.     

Atomic resolution imaging using a novel,compact and stiff scanning tunnelling microscope in cryogen-free superconducting magnet

We present the design and performance of a novel scanning tunnelling microscope (STM) operating in a cryogen-free superconducting magnet. Our home-built STM head is compact (51.5 mm long and 20 mm in diameter) and has a single arm that provides complete openness in the scanning area between the tip and sample. The STM head consists of two piezoelectric tubes (PTs), a piezoelectric scanning tube (PST) mounted on a well-polished zirconia shaft, and a large PT housed in a sapphire tube called the motor tube. The main body of the STM head is made of tantalum. In this design, we fixed the sapphire tube to the frame with screws so that the tube's position can be changed quickly. To analyse the stiffness of the STM head unit, we identified the lowest eigenfrequencies with 3 and 4 kHz in the bending modes, 8 kHz in a torsional mode, and 9 kHz in a longitudinal mode by finite element analysis, and also measured the low drift rates in the X–Y plane and in the Z direction. The high performance of the home-built STM was demonstrated by images of the hexagonal graphite lattice at 300 K and in a sweeping magnetic field from 0 T to 9 T. Our results confirm the high stability, vibration resistance, insensitivity to high magnetic fields and the application potential of our newly developed STM for the investigation of low-frequency systems with high static support stiffness in physics, chemistry, material and biological sciences.     

Observation of HOPG by STM and contact AFM in various gas atmospheres under pressures up to 1.1 MPa

Apparatus comprising a scanning tunneling microscopy (STM) and an atomic force microscopy (AFM) has been developed for use under supra-atmospheres. Observations of highly oriented pyrolytic graphite (HOPG) were carried out by STM and contact AFM operating in air and various gas atmospheres (hydrogen, helium, neon and argon) under pressures up to 1.1 MPa. Atomic resolution images of the HOPG were obtained by STM in all the gas atmospheres studied. However, it was found that the presence of water vapor gave rise to a noise current at increased pressures. Using contact AFM, the atomic resolution in an argon atmosphere decreased with increasing pressure, while atomic images were obtained under the other gas atmospheres at 1.1 MPa.     

How dry are dried samples? Water adsorption measured by STM

When operating scanning probe microscopes, like STM or AFM, under ambient conditions, the presence of water on the sample and the tip always plays an important role. The water not only influences the structure of the sample itself, but also the imaging process; in the case of the STM using a wet etched w-tip, by interfering with the electron transfer process, and in the case of the AFM, due to the capillary forces in the micro Newton range that dominate the tip surface interaction forces. In this paper, the distribution and the amount of adsorbed water on different surfaces is investigated with the help of the STM, which can provide information by imaging and by current/distance spectroscopy. Hydrophilic and hydrophobic surfaces like titanium, gold, and graphite were studied at a relative humidity between 10 and 90%. Under very dry conditions with relative humidity below 15%, the presence of water was only detectable by the longer decay length of the measured current with distance compared to samples prepared in UHV completely free of water. At less dry conditions on gold surfaces, water was found as droplets. With increasing humidity, the quantity and the size of these droplets increased until the whole surface became covered with water. Above 55% humidity, the thickness of the water film increased with increasing humidity up to several 10 nm. On titanium and graphite, water was always present in the form of closed layers growing in thickness with increasing humidity.     

A compact CCD‐monitored atomic force microscope with optical vision and improved performances

A novel CCD‐monitored atomic force microscope (AFM) with optical vision and improved performances has been developed. Compact optical paths are specifically devised for both tip‐sample microscopic monitoring and cantilever's deflection detecting with minimized volume and optimal light‐amplifying ratio. The ingeniously designed AFM probe with such optical paths enables quick and safe tip‐sample approaching, convenient and effective tip‐sample positioning, and high quality image scanning. An image stitching method is also developed to build a wider‐range AFM image under monitoring. Experiments show that this AFM system can offer real‐time optical vision for tip‐sample monitoring with wide visual field and/or high lateral optical resolution by simply switching the objective; meanwhile, it has the elegant performances of nanometer resolution, high stability, and high scan speed. Furthermore, it is capable of conducting wider‐range image measurement while keeping nanometer resolution. Microsc. Res. Tech. 76:931–935, 2013. © 2013 Wiley Periodicals, Inc.     

In-situ STM studies of electrochemical underpotential deposition of Pb on Au(111)

A modified scanning tunnelling microscope (STM) has been used to observe in-situ deposition and stripping of an electrochemical film. With STM tip and sample immersed in an acid electrolyte, single atomic steps on Au(111) have been imaged during the deposition and stripping of a monolayer-thick, underpotential deposit (UPD) of Pb. Integration of the electrochemical current passed during the film deposition and evidence from the STM images themselves confirm monolayer coverage. Our images show enhanced film growth at step edges and defect sites. Observations of single plating and stripping cycles indicate that the Au substrate returns unaltered. Except for atomic resolution images of Au(111), which we have not yet achieved in an electrolyte, all types of Au surface features seen in air are reproduced under the electrolytic solution. The modifications made to our STM in order to perform in-situ electrochemical experiments are described.     

Polymers on graphite and gold: molecular images and substrate defects

Sub-monomolecular layers of a derivatized Phthalocyaninato-poly-siloxane (PCPS) and a Polydiacetylene (PDA) have been prepared on highly orientated pyrolytic graphite and gold by Langmuir-Blodgett and Langmuir-Schäfer techniques. Raman scattering and grazing-incidence-reflection infrared spectroscopy were used to characterize packing and molecular orientations within these films. It was found that PCPS forms similarly well ordered monolayers on both graphite and gold while PDA does not. Scanning tunnelling microscopy (STM) was performed in air using both the constant height and constant current mode. On highly orientated pyrolytic graphite substrates various defect structures based on a √3X√3 R 30° superstructure were found near localized defects and small graphite steps. They were carefully distinguished from molecular images of densely packed hydrocarbon chains. Defect rich graphite was characterized with both STM and Raman spectroscopy. Similarly, disordered and graphite-like regions were found on carbon fibres. The sensitivity of STM to surface defects in graphitic material turned out to be large compared to that of the Raman spectroscopic method. STM images of PCPS monolayers on graphite and gold exhibited parallel polymer rods, 2 nm apart from each other.     

Imaging of granular high-Tc thin films using a scanning tunnelling microscope with large scan range

STM images are presented in the micron scale, taken in UHV with a single-tube scanner STM with SEM control of the tip position. For calibration, a carbon grid was used from which the coupling of x and y scan axes has been determined as well as the piezo-sensitivity factors. Images taken of a YBa₂Cu₃O_7-δ, film display the granular structure of the crystallites formed during the post-evaporation annealing. A direct comparison of STM scans with SEM micrographs was made which demonstrates the complementary information obtained by the two methods. The obtained resolution is compared to the tip shape which becomes crucial for the imaging of corrugated surfaces on the micron scale. With a simple geometric model, an attempt has been made to reconstruct the surface topography from STM scans based on the knowledge of the tip shape.     

Imaging an optical disc by the combined use of scanning tunnelling microscopy and scanning electron microscopy

We present the data obtained by scanning tunnelling microscopy combined with scanning electron microscopy of the digitally encoded structure on a stamper used to fabricate optical discs. The combination allows us to focus the STM tip on a preselected spot with a precision of ?0·3 μm. The data show the superiority of STM for a more detailed characterization of shape, width, length, height and fine structure appearing on the sample. We also show the influence of tip shape on STM resolution. Simultaneous use of both microscopes is possible but high electron doses produce an insulating layer of contaminants thick enough to make STM operation impossible.     

Scanning tunnelling and atomic force microscopy performed with the same probe in one unit

The technique demonstrated here provides features of both scanning tunnelling microscopy (STM) and atomic force microscopy (AFM). The metallic probe acts to record current variations and sense forces from the same sample area simultaneously. Thus, separate images may be recorded, in registry. The collected data allows real space correlations between some electrical properties and the geometric structure of a sample surface. The same tip is used since the geometry and condition of the tip can effect the data recordings. Platinum alloys, tungsten and graphite tips have been employed successfully. An AFM lever can respond to surface contact forces, within the elastic limits of the sample, while electric current is sensed by the tip of the lever. The usefulness of this experimental procedure is tested here by an application to semiconducting samples of Ag-doped CdTe in air and in paraffin oil media.     

Scanning tunnelling engineering

The great potential for building molecular scale machines and other structures was first noted by Richard Feynman (1960). He also proposed the development of tools to construct nanoscale mechanisms and devices. The range of technology that he proposed is now called nanotechnology, a term coined by Taniguchi (1974). Emergence of STM and related technology should greatly facilitate the development of nanotechnology in the decades to come. Franks' (1987b) review of nanotechnology notes the tremendous potential of STM-derived tools for what he terms ‘scanning tunneling engineering’. However, STM technology can also augment the ‘bottom up’ approaches to nanotechnology, exemplified for example by Forrest Carter's (1979, 1980, 1982, 1983) proposals for building molecular electronic devices (nanocomputers) using synthetic ‘modular chemistry’ and related techniques of supramolecular chemistry (Kuhn & Mobius, 1971; Kuhn, 1983; Lehn, 1980, 1988). A multi-tip STM system integrated with an optical microscope was proposed in 1986 as a ‘nanotechnology workstation’ suitable for scanning tunnelling engineering (Schneiker & Hameroff, 1988). In this paper, we describe an overview of scanning tunnelling engineering, present concepts for nanosensors and nanoswitches, and discuss design considerations for dual tip STM. Finally, we repeat an announcement of a series of ‘Feynman’ prizes for miniature STM.     

SNOM/STM using a tetrahedral tip and a sensitive current-to-voltage converter

Scanning near-field optical microscopes (SNOM) using the tetrahedral-tip (T-tip) with scanning tunnelling microscopy (STM) distance control have been realized in transmission and reflection mode. Both set-ups used ordinary STM current-to-voltage converters allowing measurement of metallic samples. In the transmission mode, a resolution of 10 nm to 1 nm with regard to material contrast can be achieved on binary metal samples. Because of the great near-field optical potential of the T-tip with respect to the optical resolution, it is a challenging task to find out whether these results can be transferred to non-metallic sample systems as well. This paper reports on a newly designed SNOM/STM transmission mode set-up using the tetrahedral-tip. It implements a sensitive current-to-voltage converter to widen the field of measurable sample systems. Beyond this, mechanical and optical measuring conditions are substantially improved compared to previous set-ups. The new set-up provides a basis for the routine investigation of metal nanostructures and adsorbed organic monolayers at resolutions in the 10 nm range.     

An entirely enclosed scanning tunnelling microscope capable of being fully immersed in liquid helium

We present an ultrahigh‐vacuum (UHV)‐sealed high‐stability scanning tunnelling microscope (STM) that can be entirely immersed in liquid helium and readily used in a commercial Dewar or superconducting magnet. The STM head features a horizontal microscanner that can become standalone and ultrastable when the coarse approach inertial motor retracts. Low voltage is enough to operate the STM even at low temperature owing to the powerful motor. It is housed in a tubular chamber of 49 mm outer diameter, which can be pumped via a detachable valve (DV), UHV‐sealed and remain sealed after the DV is removed. The entire so‐sealed chamber can then be inserted into liquid helium, where in situ sample cleavage is done via vacuum bellow. This allows sample cleavage and STM measurements to take place in better UHV with higher cooling power. Quality atomic resolution images of graphite and charge density wave on 1T‐TiSe₂ taken in ambient and 14 K conditions, respectively, are presented.