An ultrahigh vacuum fast-scanning and variable temperature scanning tunneling microscope for large scale imaging

We describe the design and performance of a fast-scanning, variable temperature scanning tunneling microscope (STM) operating from 80 to 700 K in ultrahigh vacuum (UHV), which routinely achieves large scale atomically resolved imaging of compact metallic surfaces. An efficient in-vacuum vibration isolation and cryogenic system allows for no external vibration isolation of the UHV chamber. The design of the sample holder and STM head permits imaging of the same nanometer-size area of the sample before and after sample preparation outside the STM base. Refractory metal samples are frequently annealed up to 2000 K and their cooldown time from room temperature to 80 K is 15 min. The vertical resolution of the instrument was found to be about 2 pm at room temperature. The coarse motor design allows both translation and rotation of the scanner tube. The total scanning area is about 8 x 8 microm(2). The sample temperature can be adjusted by a few tens of degrees while scanning over the same sample area.     

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.     

Infrared scanning microscope with high spatial resolution

Technical parameters and possible applications of an infrared scanning microscope with a spatial resolution of up to 3 μm are considered. It is shown that the device works with both array and linear photodetectors. Original PC software was designed to control the scanning process interactively and receive and process images of objects in the infrared range,.     

Refined tip preparation by electrochemical etching and ultrahigh vacuum treatment to obtain atomically sharp tips for scanning tunneling microscope and atomic force microscope

A modification of the common electrochemical etching setup is presented. The described method reproducibly yields sharp tungsten tips for usage in the scanning tunneling microscope and tuning fork atomic force microscope. In situ treatment under ultrahigh vacuum (p ≤10(-10) mbar) conditions for cleaning and fine sharpening with minimal blunting is described. The structure of the microscopic apex of these tips is atomically resolved with field ion microscopy and cross checked with field emission.     

Ultra compact multitip scanning tunneling microscope with a diameter of 50 mm

We present a multitip scanning tunneling microscope (STM) where four independent STM units are integrated on a diameter of 50 mm. The coarse positioning of the tips is done under the control of an optical microscope or scanning electron microscopy in vacuum. The heart of this STM is a new type of piezoelectric coarse approach called KoalaDrive. The compactness of the KoalaDrive allows building a four-tip STM as small as a single-tip STM with a drift of less than 0.2 nm/min at room temperature and lowest resonance frequencies of 2.5 kHz (xy) and 5.5 kHz (z). We present as examples of the performance of the multitip STM four point measurements of silicide nanowires and graphene.     

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.     

Ultrahigh vacuum, variable temperature, dual scanning tunneling microscope system operating under high magnetic field

We present a dual scanning tunneling microscope (DSTM) system operating between 2.2 K and room temperature, in a split-coil superconducting magnetic field up to 12 T and in ultrahigh vacuum. The DSTM consists of two compact STMs, each having x, y, and z coarse positioning piezoelectric steppers with embedded capacitive positioning sensor for navigation. Each STM can be operated independently and can achieve atomic resolution. The DSTM and the sample is configured in a way that allows the magnetic field orientation to be varied continuously from normal to parallel to the sample surface. Together with the sample, the DSTM can form a nanometer scale three terminal setup for transport measurement.     

Highly precise and compact ultrahigh vacuum rotary feedthrough

The precision and rigidity of compact ultrahigh vacuum (UHV) rotary feedthroughs were substantially improved by preparing and installing an optimal crossed roller bearing with mounting holes. Since there are mounting holes on both the outer and inner races, the bearing can be mounted directly to rotary and stationary stages without any fixing plates and housing. As a result, it is possible to increase the thickness of the bearing or the size of the rolling elements in the bearing without increasing the distance between the rotating and fixing International Conflat flanges of the UHV rotary feedthrough. Larger rolling elements enhance the rigidity of the UHV rotary feedthrough. Moreover, owing to the structure having integrated inner and outer races and mounting holes, the performance is almost entirely unaffected by the installation of the bearing, allowing for a precise optical encoder to be installed in the compact UHV rotary feedthrough. Using position feedback via a worm gear system driven by a stepper motor and a precise rotary encoder, the actual angle of the compact UHV rotary feedthrough can be controlled with extremely high precision.     

A scanner for an ultrahigh-vacuum low-temperature scanning tunneling microscope

A scanner for an ultrahigh-vacuum low-temperature scanning tunneling microscope is described. It has a high resonance frequency (>30 kHz) and a small thermal-drift rate (≤1 nm/°C) at room temperature. The scanner feeds the tip to the sample at a distance of up to 3 mm and positions it in the sample plane on a 4 × 4-mm area. These characteristics of the scanner allow one to study atomic structures at temperature variations from 5 to 300 K with objects under study remaining in view of the microscope. The scanner has a horizontal attachment for a sample with a size of up to 6 × 6 × 3mm and ensures a scanning field of 4.8 × 4.8 × 0.6 μm at 300 K and 0.8 × 0.8 × 0.1 μm at 5 K, as well as the possibility of heating to 150°C and easily replacing the sample and tip with vacuum manipulators.     

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.     

Biological structures imaged in a hybrid scanning transmission electron microscope and scanning tunneling microscope

A hybrid scanning transmission electron microscope (STEM) and scanning tunneling microscope (STM) is described which allows simultaneous imaging of biological structures adsorbed to electron-transparent specimen supports in both modes of scanning microscopy, as demonstrated on uncoated phage T4 polyheads. We further discuss the reproducibility and validity of height data obtained from STM topographs of biomacromolecules and present raw data from topographs of freeze-dried, metal-coated nuclear envelopes from Xenopus laevis oocytes.     

A compact STED microscope providing 3D nanoscale resolution

The advent of supercontinuum laser sources has enabled the implementation of compact and tunable stimulated emission depletion fluorescence microscopes for imaging far below the diffraction barrier. Here we report on an enhanced version of this approach displaying an all-physics based resolution down to (19 ± 3) nm in the focal plane. Alternatively, this single objective lens system can be configured for 3D imaging with resolution down to 45 × 45 × 108 nm in a cell. The obtained results can be further improved by mathematical restoration algorithms. The far-field optical nanoscale resolution is attained in a variety of biological samples featuring strong variations in the local density of features.     

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.     

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.     

A low temperature scanning tunneling microscope for electronic and force spectroscopy

In this article, we describe and test a novel way to extend a low temperature scanning tunneling microscope with the capability to measure forces. The tuning fork that we use for this is optimized to have a high quality factor and frequency resolution. Moreover, as this technique is fully compatible with the use of bulk tips, it is possible to combine the force measurements with the use of superconductive or magnetic tips, advantageous for electronic spectroscopy. It also allows us to calibrate both the amplitude and the spring constant of the tuning fork easily, in situ and with high precision.     

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.     

Development of a high energy resolution electron energy-loss spectroscopy microscope

We have developed a high energy resolution electron energy-loss spectroscopy (EELS) microscope, which can take spectra from specified small specimen areas and specified small reciprocal space areas to investigate detailed electronic structures. The EELS microscope is equipped with retarding Wien filters as the monochromator and the analyser. The filters are designed to achieve a stigmatic focus. The energy resolutions are 12 meV and 25 meV for cases without and with a specimen, respectively. Spatial and momentum resolutions are 30–110 nm in diameter and 1.1 nm⁻¹ in angular diameter, respectively. EELS spectra are presented to show the performance of this instrument.     

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.     

Tip-enhanced near-field Raman spectroscopy with a scanning tunneling microscope and side-illumination optics

Conventional Raman spectroscopy (RS) suffers from low spatial resolution and low detection sensitivity due to the optical diffraction limit and small interaction cross sections. It has been reported that a highly localized and significantly enhanced electromagnetic field could be generated in the proximity of a metallic tip illuminated by a laser beam. In this study, a tip-enhanced RS system was developed to both improve the resolution and enhance the detection sensitivity using the tip-enhanced near-field effects. This instrument, by combining RS with a scanning tunneling microscope and side-illumination optics, demonstrated significant enhancement on both optical sensitivity and spatial resolution using either silver (Ag)-coated tungsten (W) tips or gold (Au) tips. The sensitivity improvement was verified by observing the enhancement effects on silicon (Si) substrates. Lateral resolution was verified to be below 100 nm by mapping Ag nanostructures. By deploying the depolarization technique, an apparent enhancement of 175% on Si substrates was achieved. Furthermore, the developed instrument features fast and reliable optical alignment, versatile sample adaptability, and effective suppression of far-field signals.