Study of the fractal character of surfaces by scanning tunnelling microscopy: Errors and limitations

The possibility of using the intrinsic three-dimensional imaging capability of scanning tunnelling microscopes to study the fractal character of surfaces by Mandelbrot's method of ‘filling’ with water up to a given height is discussed. By plotting on a log-log plot the area against the perimeter of the ‘lakes' that appear, the fractal dimension is obtained from the slope of the straight line fitting the data points. The possible errors and limitations of the method are discussed from results obtained from both simulated and real surfaces. The effect of noise and resolution in the scanning tunnelling microscope on the calculation of the fractal dimension is also discussed.     

Arsenic-terminated silicon and germanium surfaces studied by scanning tunnelling microscopy

The epitaxial growth of As on the (111) and (100) faces of Si and the (111) face of Ge has been studied with vacuum tunnelling microscopy. The (111) faces of both semiconductors display a principally 1×1 termination, but differ with the presence of point defects on the Si(111): As-1×1 surface and trenches separating large (～ 100 Å) domains on the Ge(111): As-1×1 surface. I-V characteristics of the tunnel junction show a surface energy gap of approximately 1·9 eV for the Si(111): As-1×1 surface and 0·9 eV for the Ge(111): As-1×1 surface, in good agreement with recent theoretical calculations for these systems. As deposition on Si(001) results in a nominal 2×1 reconstruction of symmetric As dimers and elimination of missing dimer defects characteristic of the native Si(001) 2×1 surface. Further studies on vicinal, double-stepped substrates shows the orientation of the dimers with respect to the substrate depends critically on the substrate temperature during the growth phase, with destruction of the single principle domain surface order occurring at temperatures in excess of 700°C.     

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).     

Fractal characterization by frequency analysis: III. Effect of noise

The effect of noise in the fractal characterization by frequency analysis of surface images obtained by scanning tunnelling microscopy (STM), atomic force microscopy (AFM) or profilometry has been studied. The origin of noise and its relationship to the signal is discussed. A procedure to simulate noisy images is presented. From the study it is concluded that the method usually used to characterize noise in STM is not valid and it is shown that fractal characterization of surfaces when noise is present by traditional frequency analysis methods is not possible. A new method to perform both the noise characterization and the fractal characterization of surfaces when noise is present is proposed.     

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.     

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.     

Optimal and near-optimal filters in high-resolution electron microscopy

Two filters for improving the visibility of crystalline material in the presence of amorphous surface contamination layers in high-resolution electron microscope images can be constructed automatically from the information present in the Fourier transform of the recorded image. The recorded signal is considered in the first approximation to be the sum of two signals which are uncorrelated in the frequency domain. By estimating the power spectrum of the signal from the amorphous layer, an optimized estimate for the desired signal is given by the Wiener filter. A second filter which uses the estimated amplitude of the amorphous signal to subtract out a background can be shown to be related to the Wiener filter. The two filters are applied to an experimental image of zeolite and the effects of the two filters are compared.     

An automatic method for atom identification in scanning tunnelling microscopy images of Fe‐chalcogenide superconductors

We describe a computational approach for the automatic recognition and classification of atomic species in scanning tunnelling microscopy images. The approach is based on a pipeline of image processing methods in which the classification step is performed by means of a Fuzzy Clustering algorithm. As a representative example, we use the computational tool to characterize the nanoscale phase separation in thin films of the Fe‐chalcogenide superconductor FeSe_xTe_1‐x, starting from synthetic data sets and experimental topographies. We quantify the stoichiometry fluctuations on length scales from tens to a few nanometres.     

Comparison in spatial spreads of secondary electron information between scanning ion and scanning electron microscopy

Monte Carlo simulations have been carried out to compare the spatial spreads of secondary electron (SE) information in scanning ion microscopy (SIM) with scanning electron microscopy (SEM). Under Ga ion impacts, the SEs are excited by three kinds of collision-partners, that is, projectile ion, recoiled target atom, and target electron. The latter two partners dominantly contribute to the total SE yield gamma for the materials of low atomic number Z2. For the materials of high Z2, on the other hand, the projectile ions dominantly contribute to gamma. These Z2 dependencies generally cause the gamma yield to decrease with an increasing Z2, in contrast with the SE yield delta under electron impacts. Most of the SEs are produced in the surface layer of about 5lambda in depth (lambda: the mean free path of SEs), as they are independent of the incident probe. Under 30 keV Ga ion impacts, the spatial spread of SE information is roughly as small as 10 nm, decreasing with an increasing Z2. Under 10 keV electron impacts, the SEI excited by the primary electrons has a small spatial spread of about 5lambda, but the SEII excited by the backscattered electrons has a large one of several 10 to several 100 nanometers, decreasing with an increasing Z2. The main cause of a small spread of SE information at ion impact is the short ranges of the projectile ions returning to the surface to escape as backscattered ions, the recoiled target atoms, and the target electrons in collision cascade. The 30 keV Ga-SIM imaging is better than the 10 keV SEM imaging in spatial resolution for the structure/material measurements. Here, zero-size probes are assumed.     

Scanning tunnelling microscopy imaging of [3 × 3] Mn nonanuclear grids

The scanning tunnelling microscopy imaging of [3 × 3] Mn(II) nonanuclear grids on gold substrates is described. Self‐assembled behaviour is observed at both high and low coverage, with submolecular resolution of individual molecules displayed at low deposition concentrations. The importance of proper image processing techniques is demonstrated in resolving the layer structure at high coverage.     

Oriented immobilization of Pseudomonas putida putidaredoxin at a gold (111)–buffer interface: a real time scanning tunnelling microscopy study

A scanning tunnelling microscopy study of adsorption of wild‐type Pseudomonas putida putidaredoxin at a gold (111)–buffer interface has been made in real time. Reversible adsorption has been observed reflecting weak interaction of the wild‐type protein with a gold (111) electrode. A genetically engineered mutant, C73S‐D58C, which contains a surface thiol, has been used for ‘immobilization’ and ‘orientated adsorption’ on the gold surface. The implication of such orientated immobilization in development of a bio‐electrode surface has been predicted.     

Force sensing in scanning tunnelling microscopy: observation of adhesion forces on clean metal surfaces

Tip sample interaction forces were investigated during normal tunnelling operation of the STM using an Ir tip and a polycrystalline Ir sample. Metallic adhesion interaction was observed for tunnel conductivity ranging from 10^?6 to 19^{?9 Ω-1} implying that the actual gap width was of the order of 1–4 Å. Similar experiments performed on a polycrystalline Al sample exposed to 1 Langmuir O₂ showed that tip sample interaction changed from attractive to repulsive on well-defined areas extending over ～100 Ų which we identified with the oxidized Al surface.     

Investigation of Si–Au vicinal surfaces using scanning tunnelling microscopy and reflection high-energy electron diffraction

Silicon vicinal surfaces can be successfully used as substrates for the preparation of one‐dimensional nanostructures. The quality of the structures prepared may be controlled using scanning tunnelling microscopy, as shown in this work. Additionally, it is possible to obtain valuable information using reflection high‐energy electron diffraction. A typical way of employing reflection high‐energy electron diffraction is to observe patterns of scattered electrons on a screen. However, it is possible to obtain more detailed information on the arrangement of atoms at the surface if azimuthal plots are collected. Azimuthal plots are measured by recording the intensity of specularly reflected electrons during the rotation of the sample around an axis perpendicular to its surface. So far, only flat surfaces have been examined in such a way. In this work, it is shown that such data, containing interesting features, can also be collected for vicinal surfaces.     

Gaussian-Taylor signal-to-noise ratio estimation for scanning electron microscope images

A new and robust parameter estimation technique, named Gaussian-Taylor interpolation, is proposed to predict the signal-to-noise ratio (SNR) of scanning electron microscope images. The results of SNR and variance estimation values are tested and compared with piecewise cubic Hermite interpolation, quadratic spline interpolation, autoregressive moving average and moving average. Overall, the proposed estimations for noise-free peak and SNR are most consistent and accurate to within a certain acceptable degree compared with the others.     

Limits of topographic measurement by the scanning tunnelling and atomic force microscopes

Parameters describing the topographic character of a surface (height, surface wavelength, slope and curvature) can be derived from equivalent sinusoidal profiles. The response of a surface-measuring instrument may be modelled in terms of instrument parameters such as stylus radius, and scanning range and resolution. The performance of the instrument may then be mapped as a zone in amplitude-wavelength (AW) space to show the sinusoidal profiles it is capable of measuring. In a first-order analysis the STM and AFM are considered as equivalent to contact-stylus instruments with a notional stylus radius equal to the tip radius plus the gap. Comparisons between different instruments and types of instrument are readily made by mapping in AW space. The error arising from convolution of the sinusoidal profile with that of the finite tip may be quantified and plotted as contours in AW space.     

The tetrahedral tip as a probe for scanning near-field optical microscopy at 30 nm resolution

The tetrahedral tip is introduced as a new type of a probe for scanning near-field optical microscopy (SNOM). Probe fabrication, its integration into a scheme of an inverted photon scanning tunnelling microscope and imaging at 30 nm resolution are shown. A purely optical signal is used for feedback control of the distance of the scanning tip to the sample, thus avoiding a convolution of the SNOM image with other simultaneous imaging modes such as force microscopy. The advantages of this probe seem to be a very high efficiency and its potential for SNOM at high lateral resolution below 30 nm.     

Reproducibility and accuracy of spatial measurements from digitally captured images in the environmental scanning electron microscope

Accurate spatial measurements in a scanning electron microscope (SEM) require calibration of the magnification as a function of working distance and microscope operating conditions. This work presents the results of the calibration of an environmental SEM for the accurate spatial measurement of dimensions and areas in experiments, both for the measurement of strain in steel specimens under applied loads and the measurement of dimensional changes in timber with changes in relative humidity.     

Adaptive tuning piecewise cubic Hermite interpolation with Wiener filter in wavelet domain for scanning electron microscope images

Image processing is introduced to remove or reduce the noise and unwanted signal that deteriorate the quality of an image. Here, a single level two‐dimensional wavelet transform is applied to the image in order to obtain the wavelet transform sub‐band signal of an image. An estimation technique to predict the noise variance in an image is proposed, which is then fed into a Wiener filter to filter away the noise from the sub‐band of the image. The proposed filter is called adaptive tuning piecewise cubic Hermite interpolation with Wiener filter in the wavelet domain. The performance of this filter is compared with four existing filters: median filter, Gaussian smoothing filter, two level wavelet transform with Wiener filter and adaptive noise Wiener filter. Based on the results, the adaptive tuning piecewise cubic Hermite interpolation with Wiener filter in wavelet domain has better performance than the other four methods.