A new method of scanning tunneling spectroscopy for study of the energy structure of semiconductors and free electron gas in metals

In this study, anew method for the scanning tunneling spectroscopy (STS) of direct and indirect gap semiconductors and free electron gas in metals is proposed. Band structures of Si, porous Si, and Ge were studied. The tunneling current-voltage characteristics of Si and porous Si surfaces were measured over different voltage intervals from tens of mV to 20 V under incident light from an Xe lamp and those of a Ge surface in the dark. The correlation between the shapes of the I-V curves and band structure of the materials was calculated. It was found that the curves are linear if measured in the voltage range V₀ E_g/(2e) and nonlinear when V₀ α E_g/(2e) (in the measurements the applied voltage was changed from -V₀ to V₀). The method was used for the observation of a new effect of tunneling of free electron gas having thermal energies from a metal tip to a band gap state of the semiconductor. The energy spectrum of free electron gas was measured.     

扫描隧道探针的制备研究

本文概述针尖对扫描隧道显微镜的重要性,总结制备探针的各种技术,并着重介绍电化学腐蚀制备钨和铂铱合金探针的原理及电路设计。     

Combining scanning tunneling microscopy and synchrotron radiation for high-resolution imaging and spectroscopy with chemical, electronic, and magnetic contrast

The combination of high-brilliance synchrotron radiation with scanning tunneling microscopy opens the path to high-resolution imaging with chemical, electronic, and magnetic contrast. Here, the design and experimental results of an in-situ synchrotron enhanced x-ray scanning tunneling microscope (SXSTM) system are presented. The system is designed to allow monochromatic synchrotron radiation to enter the chamber, illuminating the sample with x-ray radiation, while an insulator-coated tip (metallic tip apex open for tunneling, electron collection) is scanned over the surface. A unique feature of the SXSTM is the STM mount assembly, designed with a two free-flex pivot, providing an angular degree of freedom for the alignment of the tip and sample with respect to the incoming x-ray beam. The system designed successfully demonstrates the ability to resolve atomic-scale corrugations. In addition, experiments with synchrotron x-ray radiation validate the SXSTM system as an accurate analysis technique for the study of local magnetic and chemical properties on sample surfaces. The SXSTM system's capabilities have the potential to broaden and deepen the general understanding of surface phenomena by adding elemental contrast to the high-resolution of STM.     

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.     

Observation of removal of an Fmoc protecting group by scanning tunneling microscopy

We demonstrate here by imaging successive surface reactions in self-assembled monolayers (SAMs) on Au(1 1 1) at molecular scale with a scanning tunneling microscope (STM): (i) SAM matrices formation with 1-octanethiol on Au(1 1 1) in ethanol, (ii) insertion of N-Fmoc-aminooctanethiol into the SAM matrices in ethanol, and (iii) removal of the Fmoc protecting group with tris(2-aminoethyl)amine (TAEA). The total reaction is formation of SAMs containing a small amount of NH₂ terminated molecules in the CH₃ terminated SAM matrices. After the reaction of the protecting group with TAEA, STM imaging revealed the decrease in heights of the inserted molecules on average. We attributed this observation to removal of the protecting group by taking account of a convolution of electronic and topographic contributions to observed STM heights. Apparent areas of the terminal groups, however, became larger on removal. The increase in the areas was attributed to water adsorption to the NH₂ terminal group under air.     

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.     

Bridging the gap between conventional and video-speed scanning probe microscopes

A major disadvantage of scanning probe microscopy is the slow speed of image acquisition, typically less than one image per minute. This paper describes three techniques that can be used to increase the speed of a conventional scanning probe microscope by greater than one hundred times. This is achieved by the combination of high-speed vertical positioning, sinusoidal scanning, and high-speed image acquisition. These techniques are simple, low-cost, and can be applied to many conventional microscopes without significant modification. Experimental results demonstrate an increased scan rate from 1 to 200 Hz. This reduces the acquisition time for a 200×200 resolution image from 3 min to 1 s.     

Analytical scanning electron microscopy for solid surface

A scanning electron microscope of ultra-high-vacuum (UHV-SEM) with a field emission gun (FEG) is operated at the primary electron energies of from 100 eV to 3 keV. The instrument can form the images that contain information on surface chemical composition, chemical bonding state (electronic structure), and surface crystal structure in a microscopic resolution of several hundred angstroms (Å) using the techniques of scanning Auger electron microscope, scanning electron energy loss microscope, and scanning low-energy electron diffraction (LEED) microscope. A scanning tunneling microscope (STM) also has been combined with the SEM in order to obtain the atomic resolution for the solid surface. The instrumentation and examples of their applications are presented both for scanning LEED microscopy and STM.     

Detection of human serum albumin on protein array using scanning tunneling microscopy

Electrical detection of biological binding events, such as protein–protein interaction and DNA hybridization, has emerged as an alternative method to conventional colorimetric and fluorescence based methods. In this study, we demonstrate an electrical detection technique of protein array which can be simply extended for multifunctional measurements and detection of biological binding events on micro-scale array. Micro-contact technique was used for the fabrication of protein chip. The fabricated protein array on Au substrate was characterized by fluorescence microscopy and scanning tunneling microscopy (STM). The chip was designed to investigate immunocomplexes comprised of our model protein, human serum albumin (HSA), corresponding antibody fragments, and Au nanoparticle–antibody conjugates. The peak-like pulse obtained by electrical tunneling current between these complexes and the STM tip varies on the surface density of the bound complexes. Using the electrical detection technique based on STM, 100 fg/mL of HSA could be successfully detected by STM. Importantly, the proposed concept of measurement could allow multiple analyses of analytes at nano-scale array, which is difficult to be analyzed by conventional fluorescence based method.     

A low-temperature scanning tunneling microscopy investigation of single electron effects

The design and the performance of a low-temperature scanning tunneling microscope (STM) operating in ultrahigh vacuum (UHV) is described. The sample and the STM are cooled by means of a helium bath cryostate. The STM consists of a “beetle”-type microscope, which is mounted on a spring suspension stage that can be operated between room temperature and 30 K. We present the results of tunneling spectroscopy on ligand-stabilized Au₅₅-clusters on a thiol-covered gold substrate. I(V)-curves taken at 100 K clearly show coulomb staircase structures, which agree well with theoretical predictions for these structures.     

Scanning tunneling microscopy of Fe- and O-sublattices on Fe3O4(100)

We present scanning tunneling microscopy of an octahedral (B) plane terminated (square root of 2 x square root of 2) R45 degrees-reconstructed surface of a natural magnetite (100) crystal. Implementing a W-tip we achieve the same resolution on Fe rows as was reported in the past either with the use of antiferromagnetic tips or on magnetite (Fe3O4) films. We show images of Fe or O sublattices of Fe3O4 with atomic resolution.     

A compact sensor head for simultaneous scanning force and near-field optical microscopy

A compact sensor head based on scanning force microscopy (SFM) using cantilever probes has been developed. The idea is to replace the microscope objective of a conventional optical microscope by this compact module and turn the optical microscope into a scanning force and near-field optical microscope with subwavelength resolution. We describe our concept and present initial results showing images of the object’s optical properties and surface topography recorded simultaneously.     

Photon scanning tunneling microscope,now and in the future

The concept of photon tunneling and the principle of the photon scanning tunneling microscope (PSTM) are described. The history of the PSTM and its development in China are reviewed. The principal problem in the recent development of the PSTM, together with its solution, is discussed. The distinguishing features and the future of the PSTM are described.     

Resolution in nonlinear laser scanning microscopy

The lateral and depth resolution of nonlinear microscopy was studied systematically. Nonlinear microscopy can be classified into several categories depending on the coherence properties of the process that generates the imaging signal from the illuminating light, on whether a single- or a two-beam geometry is used, and whether the optical setup is Type I or Type II. An evaluation of the imaging equations shows that (i) lateral and depth resolution improve with increasing nonlinearity, (ii) the differences between coherent and incoherent imaging diminish, and (iii) nonlinear imaging allows depth discrimination in Type I microscopy.     

Characterising the surface and interior chemistry of core-shell nanoparticles using scanning transmission electron microscopy

A method for extracting core and shell spectra from core-shell particles with varying core to shell volume fractions is described. The method extracts the information from a single EELS spectrum image of the particle. The distribution of O and N was correctly reproduced for a nanoparticle with a TiN core and Ti-oxide shell. In addition, the O distribution from a nanoparticle with a Cu core and a Cu-oxide shell was obtained, and the extracted Cu L_2,3-core and shell spectra showed the required change in EELS near edge fine structure. The extracted spectra can be used for multiple linear least squares fitting to the raw data in the spectrum image. The effect of certain approximations on numerical accuracy, such as treating the nanoparticle as a perfect sphere, as well as the intrinsic detection limits of the technique have also been explored. The technique is most suitable for qualitative, rather than quantitative, work.     

Spatially resolved low-temperature spectroscopy on niobium bulk samples

Using a low-temperature STM, simultaneous measurements of the surface topography and of spatial variations in the current-voltage characteristics have been performed on poly-crystalline niobium bulk samples. A special electronic set-up was developed which allows the tip bias to be swept at a constant tip position. From the resulting I(V) curves the actual magnitude of the superconducting energy gap is derived. The comparison of the surface morphology and gap distribution permits the detection of possible correlations between local variations in the superconductivity and in the topography. Upon the application of an external magnetic field, local variations of the gap are observed which have no topographic counterparts. This latter observation might indicate the existence of isolated vortices.     

Probing large area surface plasmon interference in thin metal films using photon scanning tunneling microscopy

The interference of surface plasmons can provide important information regarding the surface features of the hosting thin metal film. We present an investigation of the interference of optically excited surface plasmons in the Kretschmann configuration in the visible spectrum. Large area surface plasmon interference regions are generated at several wavelengths and imaged with the photon scanning tunneling microscope. Furthermore, we discuss the non-retarded dispersion relations for the surface plasmons in the probe–metal system modeled as confocal hyperboloids of revolution in the spheroidal coordinate systems.     

Scanning tunnelling microscopy and spectroscopy on Cu(111) and Au(111)

We have studied Cu(111) and Au(111) by means of scanning tunnelling microscopy and spectroscopy. The constant current topographies showed flat parts as well as regions with a high density of monoatomic steps (in particular on Au(111)). Local I/U characteristics have been determined at a fixed sample-tip distance in the range of ?10 V≤U≤10 V. They show a linear behaviour near the Fermi level and a nearly exponential dependency for larger values of U. Neither an influence of the sp-like surface states or an onset due to d electron contributions of the sample could be observed.     

Dynamics of annular bright field imaging in scanning transmission electron microscopy

We explore the dynamics of image formation in the so-called annular bright field mode in scanning transmission electron microscopy, whereby an annular detector is used with detector collection range lying within the cone of illumination, i.e. the bright field region. We show that this imaging mode allows us to reliably image both light and heavy columns over a range of thickness and defocus values, and we explain the contrast mechanisms involved. The role of probe and detector aperture sizes is considered, as is the sensitivity of the method to intercolumn spacing and local disorder.     

Fabrication of hierarchical micro/nanostructures via scanning probe lithography and wet chemical etching

In this study, we propose a simple and effective method for fabricating hierarchical silicon structures via the combination of scanning probe lithography (SPL) and wet chemical etching. Here, silicon oxide structures were protruded from a 100-oriented silicon surface, followed by the passivation of silicon nitride by AFM tip-induced local oxidation. Based on the two-dimensional (2D) silicon oxide patterns, three-dimensional (3D) microstructures with high aspect ratios were formed by wet etching with HF and KOH. A variety of combinations of SPL and the etching process allowed us to fabricate diverse silicon-based structures such as deep-etched microstructures and multi-terraced nanostructures.