Lateral resolution of the scanning tunnelling microscope

A theoretical study of the current distribution in a model which extracts the prominent characteristics of a tip-surface geometry in a scanning tunnelling microscope is presented. The sample is a Sommerfeld metal with a planar surface while the tip, also made of a Sommerfeld metal with a planar surface, presents a hemispherical protrusion. Schrödinger's equation is solved by using a form of the finite element method suitable to treat the three-dimensional tunnelling problem. We have derived the current distribution for several values of the protrusion radius and for various gaps between the electrodes. From these results, we investigate the ideal resolution of the scanning tunnelling microscope for realistic values of these geometrical parameters. Though applied to a rather simple model, at this stage, our method appears to be a suitable scheme for further, more refined computations, accounting for the detailed atomic structure of the electrodes.     

Real-time scanning tunnelling microscopy of surfaces under active electrochemical control

A scanning tunnelling microscope has been designed which allows tunnelling microscopy to be performed in the presence of an externally applied electrochemical current. Separate, isolated electrodes were used for electrochemical control, and up to 1 mA was passed during real-time, video-rate, in situ STM observation of the surfaces, without interfering with the operation of the STM. The noise level of these STM images is only slightly higher than images taken with the electrochemical circuitry disconnected. Surfaces were observed during the formation of surface films in aqueous electrolytes.     

Study of Au surfaces by scanning tunnelling microscopy

The reconstructions of Au surfaces have been studied by scanning tunnelling microscopy. Topographs of Au(110)-(1×2) as a function of annealing temperature show changes in the long range order, in good agreement with diffraction measurements and theoretical studies. Some insight into the nucleation and growth of the (1×2) reconstruction was obtained by imaging the surface after deposition of Cs or O. A new structural model for Au(100)-(5×20) is proposed with a high resolution topograph. Adsorption of Si clusters on Au(100) will be described.     

Safe fabrication of sharp gold tips for light emission in scanning tunnelling microscopy

Gold is the optimal tip metal for light emission in scanning tunnelling microscopy (LESTM) under ambient conditions. Sharp Au-tips of 10 nm radius were produced reliably using a safe, two-step etching method in 20% (w/w) CaCl₂ solution. Previous CaCl₂-based methods have tended to produce blunter tips, while other etching techniques that do produce sharp Au-tips, do so with the use of toxic or hazardous electrolytes. The tips are characterised using scanning electron microscopy and their efficacy in LESTM is evidenced by high-resolution, simultaneous topographic and photon mapping of Au(1 1 1)- and polycrystalline Au-surfaces. Spectra of the optical emission exhibit only one or two peaks with etched tips in contrast to the more complex spectra typical of cut tips; this feature, together with the highly symmetric geometry of the tips, facilitates a definitive analysis of the light emission process.     

Observation of rhombic facets on platinum wire after heating in air using scanning tunnelling microscopy

Evidence is provided for the formation of surface faceting due to heating in air at 1160 K. For the first time diamond-shaped facets with angles of 60 and 120° have been observed on the surface of a sample of ultrapure platinum wire in air using scanning tunnelling microscopy. The maximum extension of the facets is about 1000 Å.     

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 microscopy of oxidized graphite

Scanning tunnelling microscopy (STM) and transmission electron microscopy (TEM) have been used to investigate the surface of a pyrolitic graphite oxidized in liquid phase by NaClO. Two main features of the oxidized HOPG are revealed by STM. First, a large number of steps of different heights have developed on the graphite surface. These steps can be observed by TEM on another kind of graphite, HSAG 12, but this technique cannot give any information on their heights. Another kind of defect on the previously flat surface of HOPG consists in patches where the surface is rough and perturbed. These domains are very difficult to observe by TEM due to a poor contrast. Thus for the study of surface heterogeneities intentionally created on graphite, STM, providing information along three directions, appears to be complementary of TEM which gives only images of project area.     

Supported metal model catalyst surfaces examined by scanning tunnelling microscopy

Topographic and/or barrier-height images of ultrafine Pt and Au metal particles supported on a vacuum-deposited carbon film or titanium oxide thin films grown on titanium metal sheets were obtained. The topographic images of colloidal Au particles (5-nm diameter) adsorbed on a titanium oxide thin film showed a structure elongated in the direction normal to the x scan, indicating their weak interaction with the support surface. The topographic images of Pt vacuum-deposited on a carbon film showed c. 4-nm diameter particles, larger than those observed in electron microscopy. The problems inherent to the STM observation of such dispersed metal systems are identified. In the case of Pt particles vacuum-deposited on titanium oxide film, its barrier-height image gave better indication of different phases on the surface than its topographic image. The significance of obtaining barrier-height images along with topographic images for such sample systems is demonstrated.     

Anomalous voltage dependence of tunnelling microscopy in WSe2

We present scanning tunnelling microscopy (STM) investigations of the layered semiconductor WSe₂. The tunnelling experiments were performed in air and under silicone oil with markedly different results. In air, atomic resolution images of the hexagonally structured surface could be obtained for sample-to-tip voltages of both negative and positive polarities, from ?1·5 to ?0·3 V for negative sample and from +0·6 to +1·6 V for positive sample, respectively. Under silicone oil, however, good atomic images could be seen for negative sample biases down to at least ?14 V, while for positive sample biases no difference with respect to the tunnelling in air was found.     

Scanning tunnelling microscopy of 1-D and 2-D charge-density wave systems

We have used a new variable temperature scanning tunnelling microscope (STM) to study quasi-1D and 2-D charge-density wave (CDW) systems. The 1-D systems, typified by NbSe₃ and TaS₃, are of special interest since they exhibit unusual transport phenomena associated with moving CDW above a threshold electric field. In the case of NbSe₃, room temperature STM images show both major and subtle details of the lattice structure. At present, however, images taken below the Peierls transition temperature of T_P=144 K resolve major lattice details but are not sufficiently clear to resolve the CDW. On the other hand, for the fully gapped CDW system orthorhombic-TaS₃, the CDW modulation superimposed on the lattice structure and having the correct period of four times the S-S spacing of 3·3 Å, is observed below T_P=215 K. Above T_P, the main observable feature is the S-S spacing along the chains. STM measurements have also been performed on the 2-D CDW system 1T-TaS₂ in its incommensurate, nearly commensurate, fully commensurate and trigonal phases. For the nearly commensurate phase, STM images show uniform commensurability with a relatively low concentration of small, time-varying discommensurations in contrast to models pradicting a regular domain structure. In the trigonal phase, however, evidence is seen for the striped phase composed of long, nearly parallel discommensurations.     

Scanning tunnelling microscopy of charge density waves in 1T-TaS2

Using a variable temperature scanning tunnelling microscope we have observed both the lattice and the triple charge density wave (CDW) in 1T-TaS₂. We obtained images of the nearly-commensurate (NC) phase between 350 and 200 K and the triclinic (T) phase between 220 and 280 K. We analysed the images to determine the local angle of rotation of the CDW relative to the lattice to determine if commensurate domains exist in this material. In the NC phase we do not see the hexagonal discommensurate domains proposed by Nakanishi el al. (1977), but observe a structure which is uniformly incommensurate. The orientation of the CDW relative to the lattice is observed to be locally incommensurate and to vary continuously with temperature as reported by Scruby et al. (1975). However, in the T phase we observe long narrow commensurate domains very similar to those described by Nakanishi and Shiba (1984) for this phase.     

A scanning tunnelling microscopy study of the formation and chemical activation of step defects on the basal plane of pyrolytic graphite

Scanning tunnelling microscopy is used to monitor etching of the basal plane of highly orientated pyrolytic graphite by ozone, oxygen and nitric acid. These treatments are seen to produce numerous single and multilayer step defects. Subsequent modification of the graphite sheet edges flanking these cavities by cyanuric chloride, TiCl₄ and other reagents is shown to activate the edges, thereby making them capable of covalently binding various molecules.     

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.     

A scanning tunnelling microscope for operation in air

In this paper a scanning tunnelling microscope for operation in air is described with emphasis on the coarse and fine sample positioning mechanism, piezoelectric scanner and vibration isolation. Line scan (amplitude modulation), top view (brightness modulation) and combined shaded topographical images of the surface of highly orientated pyrolitic graphite are shown.     

Images of 16S ribosomal RNA by scanning tunnelling microscopy

We report the use of scanning tunnelling microscopy (STM) to study surface topographies of complex nucleic acid structures. From low-resolution STM images of uncoated 16S ribosomal RNA, we demonstrate the possibility of determining several objective parameters (molecular mass and radius of gyration) in order to characterize and identify the molecules observed. These parameters were compared with values obtained by other physical methods and the radius of gyration was found to be the most reliable. At high resolution, it was possible to measure the main dimensions of selected V-form particles more precisely than with electron microscopy. Images of the more compact form have been also obtained that show different domains in the macromolecular structure.     

Scanning tunnelling microscopy on reconstructed Si(110)

We have prepared clean surfaces of reconstructed Si(110), which showed a distinct 4×5 LEED pattern with particularly high intensity of the diffraction beams corresponding to a 2×1 periodicity of the surface. Images obtained by scanning tunnelling microscopy on the same surfaces are characterized by rows of reconstructed Si atoms along the direction. On high-resolution images, atomic subunits in a 2×5 periodicity of ideal Si(110) have been identified. By using these subunits as building blocks for both the 4×5 and the 2×1 reconstruction, a previously reported phase transition between both reconstructions may be explained by a loss of order along the direction.     

Optical characterization of probes for photon scanning tunnelling microscopy

The photon scanning tunnelling microscope is a well-established member of the family of scanning near-field optical microscopes used for optical imaging at the sub-wavelength scale. The quality of the probes, typically pointed uncoated optical fibres, used is however, difficult to evaluate in a direct manner and has most often been inferred from the apparent quality of recorded optical images. Complicated near-field optical imaging characteristics, together with the possibility of topographically induced artefacts, however, has increased demands for a more reliable probe characterization technique. Here we present experimental results obtained for optical characterization of two different probes by imaging of a well-specified near-field intensity distribution at various spatial frequencies. In particular, we observe that a sharply pointed dielectric probe can be highly suitable for imaging when using p -polarized light for the illumination. We conclude that the proposed scheme can be used directly for probe characterization and, subsequently, for determination of an optical transfer function, which would allow one to deduce from an experimentally obtained image of a weakly scattering sample the field distribution existing near the sample surface in the absence of the probe.     

Spectroscopy with scanning near-field optical microscopy using photon tunnelling mode

We have demonstrated Raman spectroscopy using scanning near-field optical microscopy (SNOM). Photon tunnelling mode was employed, in which the sample is illuminated using an attenuated total reflection (ATR) configuration and the evanescent wave perturbed by the sample is picked up by a sharpened optical fibre probe. By this experimental arrangement Raman scattering from the optical fibre probe was greatly reduced, therefore we were able to excite the sample using more intense laser light compared to the illumination mode SNOM. Raman spectra of copper phthalocyanine (CuPc) were obtained in the off-resonance condition and without using surface-enhanced Raman scattering (SERS).     

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.