High-resolution scanning electron microscopy.

The spatial resolution of the scanning electron microscope is limited by at least three factors: the diameter of the electron probe, the size and shape of the beam/specimen interaction volume with the solid for the mode of imaging employed and the Poisson statistics of the detected signal. Any practical consideration of the high-resolution performance of the SEM must therefore also involve a knowledge of the contrast available from the signal producing the image and the radiation sensitivity of the specimen. With state-of-the-art electron optics, resolutions of the order of 1 nm are now possible. The optimum conditions for achieving such performance with the minimum radiation damage to the specimen correspond to beam energies in the range 1-3 keV. Progress beyond this level may be restricted by the delocalization of SE production and ultimate limits to electron-optical performance.     

Monolayer freeze-fracture and scanning tunneling microscopy

This article reviews research on planar monolayer methods, application of the methods to analyses of transmembrane signaling, and the combination of these methods with scanning tunneling microscopy (STM). Past research has involved the development of monolayer freeze-fracture methods. These include monolayer freeze-fracture autoradiography (MONOFARG), an electron microscopic cytochemical method to analyze in-plane distributions of radioisotopes, and double-labeled membrane splitting (DBLAMS) and single-membrane monolayer splitting (SMMS), methods to analyze transmembrane distributions of native and radiolabeled proteins and lipids. Present research has focussed on using these methods to investigate mechanisms of transmembrane signaling mediated by protein kinase C (PKC), including the transbilayer distribution of the tumor promoter TPA, a lipophilic activator of PKC, and the transbilayer distribution of peripheral membrane proteins phosphorylated by PKC. Future work will involve the combination of planar sample preparation with STM. The principles and applications of biological STM are briefly reviewed and a low-resolution STM image of a planar purple-membrane monolayer is included. The combination of planar methods and STM can provide the chemical information lacking in STM images enabling microscopists to investigate biochemical phenomena at nanometer resolution.     

High-pressure scanning tunneling microscopy: tip reactions

Scanning tunneling microscopy (STM) is an ideal tool to image conducting and semiconducting surfaces with atomic resolution. The technique provides high-resolution images in vacuum or even high-pressure environments. Since STM can be operated at elevated pressures and temperatures, images can be collected in situ under catalytic conditions. In this work, we demonstrate that artifacts can be observed when imaging in situ since reactions can occur on the tip, and care should be taken when analyzing the data obtained.     

Insulated gold scanning tunneling microscopy probes for recognition tunneling in an aqueous environment

Chemically functionalized probes are required for tunneling measurements made via chemical contacts ("Recognition Tunneling"). Here, we describe the etching of gold STM probes suitable for chemical functionalization with moieties bearing thiol groups. Insulated with high density polyethylene, these probes may be used in aqueous electrolytes with sub pA leakage currents. The area of the exposed probe surface was characterized via the saturation current in an electroactive solution (0.1 M K(3)Fe(CN)(6)). Twenty five percent of the probes had an exposed region of 10 nm radius or less.     

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。     

High-resolution photon scanning tunneling microscopic investigations of NaCl crystal surfaces

Cleaved NaCl crystal surfaces were investigated with a photon scanning tunneling microscope. Steps 4 nm high and 3 nm wide could be resolved. The lateral resolution is coupled to the step height by the steepest measured slopes of about 50°. The measured stepwidth at shallow steps is noise-and slope-limited to 3 nm. The mapping of the decay coefficient of the evanescent field shows spatial inhomogeneities often coupled to the crystalline structure.     

High-resolution surface scanning electron microscopy of mineralized tissues

By using an ion-pumped SEM with high brightness gun, resolution of the order of 5 nm has been demonstrated on the mineral matrix of animal bone and tooth enamel. Measurements of collagen fibril diameter have also been obtained.     

Recent advances in atomic-scale spin-polarized scanning tunneling microscopy

The Mn3N2 (010) surface has been studied using spin-polarized scanning tunneling microscopy at the atomic scale. The principle objective of this work is to elucidate the properties and potential of this technique to measure atomic-scale magnetic structures. The experimental approach involves the use of a combined molecular beam epitaxy/scanning tunneling microscopy system that allows the study of atomically clean magnetic surfaces. Several key findings have been obtained. First, both magnetic and non-magnetic atomic-scale information has been obtained in a single spin-polarized image. Magnetic modulation of the height profile having an antiferromagnetic super-period of c = 12.14 A (6 atomic rows) together with a non-magnetic superstructure having a period of c/2 = 6.07 A (3 atomic rows) was observed. Methods of separation of magnetic and non-magnetic profiles are presented. Second, bias voltage-dependent spin-polarized images show a reversal of the magnetic modulation at a particular voltage. This reversal is clearly due to a change in the sign of the magnetic term in the tunnel current. Since this term depends on both the tip's as well as the sample's magnetic local density of states, the reversal can be caused by either the sample or the tip. Third, the shape of the line profile was found to vary with the bias voltage, which is related to the energy-dependent spin contribution from the 2 chemically inequivalent Mn sites on the surface. Overall, the results shown here expand the application of the method of spin-polarized scanning tunneling microscopy to measure atomic-scale magnetic structures.     

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.     

High-resolution field-emission scanning electron microscopy of nuclear pore complex

The nuclear pore complex (NPC) is a large macro-molecular assembly inserted into the nuclear envelope (NE). It controls the traffic of proteins, RNA, and RNA proteins between nucleus and cytoplasm. Its chemical composition and function are now intensively investigated in many organisms. To understand this unique membrane transport system, we must know the supramolecular organization of the NPC. In recent years, high-resolution field-emission scanning electron microscopy has made important contributions to our knowledge of NPC structure. It provided the first images of the complex and beautiful fish trap-like structure of its intranuclear surface, documented in this review. It also has provided the first images of a new intranuclear structure, a system of branching hollow cables connecting the nuclear interior with the NPCs at the nuclear surface. Most likely this is an intranuclear transport system, assuring efficient exchange between the nuclear interior and the NE, especially in large nuclei.     

Imaging of metal-coated biological samples by scanning tunneling microscopy

A method for imaging biological samples by scanning tunneling microscopy (STM) is presented. There are two main difficulties in imaging biological samples by STM: (1) the low conductivity of biological material and (2) finding a method of reliably depositing the sample on a flat conducting surface. The first of these difficulties was solved by coating the samples with a thin film of platinum-carbon. The deposition problem was solved by a method similar to a procedure used to deposit biological molecules onto field ion microscope (FIM) tips. STM images of bacteriophage T7 and filamentous phage fd are shown. The substrate on which the samples were absorbed was atomically flat gold. The images do not show molecular detail due to the metal coating, but the gross dimensions and morphology are correct for each type of virus. Also, the surface density of virus particles increases and decreases in the way expected when the conditions of deposition are changed. These methods allow reliable and reproducible STM imaging of biological samples.     

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.     

Scanning tunneling microscopy and spectroscopy investigations of QCA molecules

Quantum-dot cellular automata (QCA), a computation paradigm based on the Coulomb interactions between neighboring cells. The key idea is to represent binary information, not by the state of a current switch (transistor), but rather by the configuration of charge in a bistable cell. In its molecular realization, the QCA cell can be a single molecule. QCA is ideally suited for molecular implementation since it exploits the molecule's ability to contain charge, and does not rely on any current flow between the molecules. We have examined using an UHV-STM some of the QCA molecules like silicon phthalocyanines and Fe-Ru complexes on Au (111) and Si (111) surfaces, which are suitable candidates for the molecular QCA approach.     

Single-step electrochemical method for producing very sharp Au scanning tunneling microscopy tips

A single-step electrochemical method for making sharp gold scanning tunneling microscopy tips is described. 3.0M NaCl in 1% perchloric acid is compared to several previously reported etchants. The addition of perchloric acid to sodium chloride solutions drastically shortens etching times and is shown by transmission electron microscopy to produce very sharp tips with a mean radius of curvature of 15 nm.     

High-resolution scanning electron microscopy of frozen-hydrated and freeze-substituted kidney tissue

Inner surfaces and fracture faces of rabbit kidney tissue were investigated with high-resolution scanning electron microscopy using two different cryopreparation techniques: (i) for the observation of fracture faces, cryofixed tissue was fractured and coated in a cryopreparation chamber dedicated to SEM, vacuum transferred onto a cold stage and observed in the frozen-hydrated state; (ii) for the observation of inner surfaces of the nephron, water was removed after freezing and fracturing by freeze substitution and critical-point drying of the tissue. By both methods, macromolecular structures such as intramembranous particles on fracture faces and particles on inner surfaces were imaged. The latter method was used to investigate in more detail surface structures of cells in the cortical collecting duct. These studies revealed a heterogeneity of intercalated cells not described thus far.     

Characterization of nanowires and molecular switches with scanning tunneling microscopy

We consider the problem of finding the energy spectra, transmission and charge distribution on nanowires with scanning tunneling spectroscopy. Within this context, we first test the applicability of the method by comparing the output of our theory with available experimental results on In-based quantum wells patterned on nanowires. Then we study the correlation between density of states and electron transmission curves. Third, we investigate the induction of ultrafast electronic transitions due to the presence of a molecular switch or a scanning probe microscope tip.     

Vacancy island creation and coalescence using automated scanning tunneling microscopy

We demonstrate that scanning tunneling microscope tip-surface crash events can be utilized as an efficient means for the creation of predefined island configurations for diffusion studies. Using this method, islands of varying size can be created and placed in close proximity, increasing the probability of initiating and observing coalescence events. Data obtained from crash initiated events on a Ag(111) surface are presented. Relaxation time exponents extracted from these data confirm that our method gives results consistent with previous, sputter-obtained island coalescence studies. We also describe an instrument-control routine developed for these measurements that utilizes commercial imaging and off-the-shelf automation software to automate the tracking of islands or other features by the microscope.     

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.