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.     

用于纳米计量的双元扫描隧道显微镜

研制了用于纳米计量的双元扫描隧道显微镜 ,介绍了双元扫描隧道显微镜的原理和仪器系统 ,利用该系统对原子晶格图象进行扫描 ,验证了纳米计量的可行性 ,给出了部分被测样品的纳米计量结果     

Compact very low temperature scanning tunneling microscope with mechanically driven horizontal linear positioning stage

We describe a scanning tunneling microscope for operation in a dilution refrigerator with a sample stage which can be moved macroscopically in a range up to a cm and with an accuracy down to the tens of nm. The position of the tip over the sample as set at room temperature does not change more than a few micrometers when cooling down. This feature is particularly interesting for work on micrometer sized samples. Nanostructures can be also localized and studied, provided they are repeated over micrometer sized areas. The same stage can be used to approach a hard single crystalline sample to a knife and cleave it, or break it, in situ. In situ positioning is demonstrated with measurements at 0.1 K in nanofabricated samples. Atomic resolution down to 0.1 K and in magnetic fields of 8 T is demonstrated in NbSe(2). No heat dissipation nor an increase in mechanical noise has been observed at 0.1 K when operating the slider.     

Construction of a versatile ultralow temperature scanning tunneling microscope

We constructed a dilution-refrigerator (DR)-based ultralow temperature scanning tunneling microscope (ULT-STM) which works at temperatures down to 30 mK, in magnetic fields up to 6 T and in ultrahigh vacuum (UHV). Besides these extreme operation conditions, this STM has several unique features not available in other DR-based ULT-STMs. One can load STM tips as well as samples with clean surfaces prepared in an UHV environment to a STM head keeping low temperature and UHV conditions. After then, the system can be cooled back to near the base temperature within 3 h. Due to these capabilities, it has a variety of applications not only for cleavable materials but also for almost all conducting materials. The present ULT-STM has also an exceptionally high stability in the presence of magnetic field and even during field sweep. We describe details of its design, performance, and applications for low temperature physics.     

A metrological scanning force microscope

In this paper, the design, construction, and characterization of a metrological scanning force microscope (SFM) for the purposes of dimensional measurement of surface features is discussed. Using this instrument, precision measurements of engineering surfaces can be performed in air with subnanometer resolution. In this design, scanning of the specimen in the x and y planes and surface profiling in z-axis are each monitored directly by capacitance sensors. The present SFM is capable of a resolutions of approximately 0.1 nm over 15 μm range in z-axis and about 1 nm over 50 pm scanning range in x− and y-axes with a repeatability of less than 1 nm. The linearity error was measured to be within the noise level. Specimens ranging from soft polymeric films to polished zerodur are used to illustrate its metrological capability.     

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.     

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.     

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.     

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.     

Automatic bias-reduction controller for a scanning tunneling microscope

In order to protect the sample and the tip against current transients in a scanning tunneling microscope, which in most cases damages the scanned surface and the tip, when using a bias higher than 1V, we have designed a simple and low-cost circuit that limits the tunneling current. During the evolution of the current transient, when the current exceeds a pre-determined value, a fast feedback control mechanism immediately reduces the bias and prevents the current transient from developing. In addition, we designed a fast pre-amplifier that works with this controller. We have shown that this mechanism provides a better scanning image compared to a system without such a mechanism.     

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.     

Compact variable-temperature scanning force microscope

A compact design for a cryogenic variable-temperature scanning force microscope using a fiber-optic interferometer to measure cantilever deflection is presented. The tip-sample coarse approach and the lateral tip positioning are performed by piezoelectric positioners in situ. The microscope has been operated at temperatures between 6 and 300 K. It is designed to fit into an 8 T superconducting magnet with the field applied in the out-of-plane direction. The results of scanning in various modes are demonstrated, showing contrast based on magnetic field gradients or surface potentials.     

Scanning tunneling microscope spectroscopy of polymers

This paper presents theoretical results on the relationship between density of states (DOS) and scanning tunneling microscope current-voltage curves in polymers. We considered samples of linear hydrocarbons electrically grounded at one of their extremes. The other extreme is electrically connected to the microscope tip via electron tunneling through vacuum. When a voltage, V, is applied to the tip, electric current, I, flows in the tip-sample circuit. This current varies as the voltage varies and depends on the DOS to the extent that no current would flow if no electron states exist at a certain energy (or voltage). The detailed relationship between DOS and the current-voltage (I-V) curve is not known a priori. We solve the corresponding quantum problem in the context of tight binding and find that I-V reproduces accurately the resonant energy peaks of the DOS. We apply the results to 100 atom-long alkane and alkene chains and found that there is a significant voltage shift in the corresponding curves as to discriminate one structure from the other.     

A switchable cantilver for a chemically sensitive scanning force microscope

We describe a cantilever device for a novel ’Time-Of-Flight Scanning Force Microscope (TOF-SFM)’ concept that has the capability of chemical analysis. The cantilever device consists of a switchable cantilever (SC), a microfabricated extraction electrode, and a LEGO-type microstage, which combines two different systems. It allows quasi-simultaneous topographical and chemical imaging of a sample surface to be performed in the same way as with conventional scanning probe techniques. This is achieved by the micromachined SC with a bimorph actuator that provides a reasonable switching speed in comparison with mechanically operated switches. Secondly, a short tip-electrode distance to minimize the ions extraction voltage can be realized by LEGO-type microfabrication. The measured SC tip deflection is -100 μm at 35 mW, corresponding to an estimated heater temperature of -250°C. The maximum switching speed between the two modes is -10 msec, and the sensitivity ΔR/R of an integrated piezoresistive deflection sensor is -6.7× 10^-7/nm. The tip-electrode distance is only 10 μm. The TOF-SFM is currently integrated in an ultra-high-vacuum system to perform several measurements.     

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.     

Active mechanical noise cancellation scanning tunneling microscope

We present the design and performance of an active mechanical noise cancellation scanning tunneling microscope (STM). This system features two key parts: a "twin-tip" scanner and an active mechanical noise cancellation algorithm. The twin-tip scanner functions as two independent STMs which share nearly the same mechanical transfer function, allowing both STMs to sense nearly identical background mechanical noise. Based on an adaptive digital signal processing technique, the active mechanical noise cancellation algorithm applies the noise sensed by the first STM to concurrently cancel the noise in the second STM and hence allows the second STM to acquire spectroscopy with a significantly improved signal to noise ratio. This system demonstrates long-term stability of the tip-sample tunnel junction and improved spectroscopy measurement in a mechanically noisy environment.     

Modification of the sample holder for a variable temperature scanning tunneling microscope (Omicron)

The design of a sample holder for a variable temperature scanning tunneling microscope (VT STM (Omicron)) with a variable sample temperature is described. This design considerably extends the range of investigated materials whose surface structure is sensitive to low concentrations of contaminations. The device is manufactured on the basis of the components of a standard holder with the possibility of heat-treating samples in a temperature range of 100–1500 K. The working capacity of the modified sample holder was demonstrated for an example of obtaining a Si(100)?2 × 1 surface with an ultimately low concentration of structural defects.     

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.     

ASX-SM扫描电子显微镜大修技术

简要总结了ASX-SM扫描电镜大修的情况,阐述了故障的技术分析及解决措施.经过大修,最终使该设备恢复到生产需要,现已投入生产使用中.