Hillock sizes after wet etching in silicon

The formation of two- and three-dimensional hillocks is regularly observed in Si(1 1 1) steps and Si(1 0 0) during wet etching. Frequently the resulting morphology consists of hillocks scattered on a landscape of limited roughness. Recently we proposed a mean field model (MFM) in which the observed hillock-and-valley pattern is possible under steady state if hillock etching is slightly faster than valley etching. This condition implies that hillock size distributions must be an exponential decreasing function. In this work, we report a systematic study of hillock size distributions of experimental morphologies obtained under different etchant concentrations in Si(1 0 0). We found that experimental hillock size distributions are in agreement with those predicted by the MFM.     

Evolution of stress and strain relaxation of Ge and SiGe alloy films on Si(0 0 1)

The growth of Ge and SiGe alloy films on Si substrates has attracted considerable interest in the last years because of their importance for optoelectronic devices as well as Si-based high speed transistors. Here we give a short overview on our recent real time stress measurements of Ge and SiGe alloy films on Si(0 0 1) performed with a sensitive cantilever beam technique and accompanied by structural investigations with atomic force microscopy. Characteristic features in the stress curves provide detailed insight into the development and relief of the misfit strain. For the Stranski–Krastanow system Ge/Si(0 0 1) as well as for SiGe films with Si contents below 20%, the strain relaxation proceeds mainly into two steps: (i) by the formation of 3D islands on top of the Ge wetting layer; (ii) via misfit dislocations in larger 3D islands and upon their percolation.     

Atomic scale properties of interior interfaces of semiconductor heterostructures as determined by quasi-digital highly selective etching and atomic force microscopy

We report on first experiments combining quasi-digital highly selective etching and atomic force microscopy (AFM) to examine the interior interfaces of semiconductor heterostructures. Lattice matched (GaIn)As/InP heterostructures grown by metalorganic vapour-phase epitaxy (MOVPE) are taken as a model system to check the capabilities of this new method. Standard selective etchants for different material systems have been optimized in selectivity and etch rate to achieve a quasi-digital etching behaviour. In this way, the real structure of interior interfaces can be determined by AFM. We find a significant difference between the surface of the heterostructure and the interior interfaces.     

Step dynamics in relaxation of sharp corners on crystal surfaces

The dynamic behavior of steps involved in the relaxation of sharp corners in microfabricated structures on crystalline surfaces have been studied. We find that during the early stages of relaxation of slightly tapered trenches on Si(0 0 1), wide (1 1 0) terraces perpendicular to the substrate are formed near the corners of the trench sidewalls. The evolution of a step profile around the corner region, where step density abruptly changes, is analyzed using one-dimensional step models. It is found that, in case that mass transport occurs through surface diffusion, the preexisting steps on the trench sidewall are accumulated in the corner region, and extensive terraces are formed near the corners.     

Behavior of the (0 0 0 1) surface of sapphire upon high-temperature annealing

Evolution of the (0 0 0 1) α-Al₂O₃ surface morphology upon annealing was studied using atomic force microscopy. The annealing protocol included temperatures of 1200 and 1500 °C and different time. Vicinal Al₂O₃ (0 0 0 1) surfaces annealed at 1200 °C exhibit initial localized step coalescence that evolves into terrace-and-step with island morphology that persists for several hours. Annealing at 1500 °C results in initial step coalescence on a global scale, and yields a terrace-and-step morphology with an indication of step bunching after longer annealing times.     

Combined AFM and Brewster-angle analysis of gradually etched ultrathin SiO2 - Comparison with SRPES results

Two surface sensitive techniques are employed to assess both structural and optical properties of an inhomogeneous Si(1 1 1)/silicon oxide multilayer system. Upon gradual etch-back of the native silicon oxide layer, structural changes of the respective interfaces were determined by contact-mode atomic force microscopy (CM-AFM); optical data were obtained by Brewster-angle analysis (BAA) at a single wavelength. It is shown, that the sensitivity of BAA leads to the identification of an additional strained sub-surface layer that was investigated by subsequent etching experiments and following optical analysis. Inclusion of this layer and its interfaces into a multilayer model allowed precise numerical evaluation of the respective oxide thicknesses in the range between 12 Å and 2 Å. These values, obtained by combination of BAA and AFM, are in excellent agreement with results obtained by synchrotron radiation photoelectron spectroscopy (SRPES). It is furthermore shown, that the thickness resolution limit of BAA (at constant nanotopographic roughness) is well below 1 Å. A limitation of BAA single-wavelength analysis is reached when the roughness variation, in terms of an effective layer and its thickness, exceeds the oxide thickness variation.     

Surface reconstructions of the Si(100)–Ge system

The surface reconstruction of epitaxial Ge layer on Si(100) was studied with ultrahigh vacuum scanning tunneling microscopy. The surface with 0.8 ML Ge grown in the presence of a hydrogen surfactant reveals the same structures as found in chemical-vapor-deposited Ge on Si(100): (i) defective (2×1) structure at 290°C, (ii) irregular (2×N) in Ge layer and defective (2×1) in bare Si regions at 420°C, and (iii) (2×N) in Ge-covered regions and c(4×4) in bare Si regions at 570°C. The morphology of step edges does not change with temperature, implying that the c(4×4) reconstruction is anisotropic in nature.     

Understanding tapping-mode atomic force microscopy data on the surface of soft block copolymers

In this paper, we focus on better understanding tapping-mode atomic force microscopy (AFM) data of soft block copolymer materials with regard to: (1) phase attribution; (2) the relationship between topography and inside structure; (3) contrast-reversal artifacts; (4) the influence of annealing treatment on topography. The experiments were performed on the surface of poly(styrene–ethylene/butylene–styrene) (SEBS) triblock copolymer acting as a model system. First, by coupling AFM with transmission electron microscopy (TEM) measurements, the phase attribution for AFM images was determined. Secondly, by imaging an atomically flat SEBS surface as well as an AFM tip-scratched SEBS surface, it was confirmed that the contrast in AFM height images of soft block copolymers is not necessarily the result of surface topography but the result of lateral differences in tip-indentation depth between soft and hard microdomains. It was also found that there is an enlarging effect in AFM images on the domain size of block copolymers due to the tip-indention mechanism. Thirdly, based on the tip-indention mechanism, tentative explanations in some detail for the observed AFM artifacts (a reversal in phase image followed by another reversal in height image) as function of imaging parameters were given. Last, it was demonstrated that the commonly used annealing treatments in AFM sample preparation of block copolymers may in some cases lead to a dramatic topography change due to the unexpected order-to-order structure transition.     

Surface alloying and anomalous diffusion of Bi on Cu(1 1 1)

We have used Low-Energy Electron Microscopy (LEEM) to study the formation and structure of the surface alloy of Bi on the Cu(1 1 1) surface. As a function of Bi coverage we find a progression from a dilute surface alloy to a structure, which coexists with a Bi overlayer when the Bi coverage exceeds 1/3 ML. At a temperature of 401 K, an unusual formation of alloy domains is observed. The origin of this effect is traced down to the mobility of Bi adatoms, which is found to strongly depend on the Bi coverage of the surface alloy on which they reside.     

25 nm resolution single molecular fluorescence imaging by scanning near-field optical/atomic force microscopy

High-resolution single molecular near-field fluorescence images were observed by scanning near-field optical/atomic force microscopy (SNOM/AFM). We modified the SNOM/AFM for both high-resolution fluorescence imaging and high-resolution topographic imaging. The imaged fluorophore, Alexa 532, is prepared with a poly-methyl-methacrylate (PMMA) film coating. A fluorescence resolution of 25 nm was obtained with a simultaneous topographic image of a flat surface. A sample prepared with a lower PMMA concentration exhibited a rough surface in the micro area. The results for the flat surface indicated that the fluorescence resolution is worst in the rough surface sample, that the maximum fluorescence intensities for the individual fluorophore are similar, and that the decay rate is faster. Thus, we concluded that the morphological effect is an important factor in fluorescence image resolution and the apparent lifetimes of the fluorescence molecules.     

Regular step formation on concave-shaped surfaces on 6H–SiC(0 0 0 1)

A concave-shaped surface has been prepared in a 6H–SiC(0 0 0 1) substrate by mechanical grinding. As a consequence, the different crystallographic planes building up the 6H–SiC polytype are cut under continuously changing polar angles in all azimuthal directions. Through hydrogen etching, this curved surface breaks up into a whole set of surfaces vicinal to the initial 6H(0 0 0 1) orientation. The local structural reorganisation after hydrogen etching has been studied by scanning electron microscopy (SEM) and atomic force microscopy (AFM). Two types of local bond environments are present at the step edges leading to a strong anisotropy in the surface etching with hydrogen. As a result, the distribution of the terrace width and the step heights varies with the azimuthal angle and reflects the sixfold symmetry of the bulk crystal. For most azimuthal directions, an alternation of large and small terraces, separated by steps of 0.75 nm heights (height of half the 6H polytype, three bilayers) is observed and only for well defined azimuthal directions, equally spaced terraces separated by steps of 1.5 nm height (one unit cell of 6H–SiC, six bilayers) are found. In addition, the polar variations have been studied by taking various line-scans along the concave-shaped surface with AFM. It seems that for polar angles above 3°, step bunching of several SiC steps occurs whereas below 3° the bimodal terrace width distribution is observed.     

Evidence for diffusion-limited kinetics during electromigration-induced step bunching on Si(1 1 1)

We have measured how the initial terrace width l₀ on vicinal Si(1 1 1) surfaces influences the rate of step bunching and the minimum terrace width within a bunch when direct-current heated at 940-1290 °C. A comparison of this data with analytic solutions and numerical simulations of the conventional “sharp-step” model give strong evidence that the kinetic length d is relatively small (d < ∼20 nm) in both temperature regime I (∼850-950 °C) and regime III (∼1200-1300 °C), in which step-down current is required for step bunching. This indicates that surface mass transport is diffusion-limited in both regimes I and III when l₀ > 20 nm, and hence that the adatom attachment- and terrace diffusion-hopping rates are of comparable magnitude. We also observe similar scaling with initial terrace width in temperature regime II (∼1040-1190 °C), in which step-up current is required for bunching, suggesting a similar step bunching mechanism in all three temperature regimes.     

Ion-bombardment induced morphology change of device related SiGe multilayer heterostructures

Ion assisted molecular beam epitaxy bears the potential to tune morphological and structural parameters of semiconductor heterolayers for opto- and nanoelectronic applications. The morphology evolution and the degree of relaxation are influenced by the ion beam parameters and the strain of the heteroepitaxial film. In this work, the morphology of silicon germanium (SiGe) layers due to Si⁺-ion beam treatment during growth is investigated by atomic force microscopy (AFM) as a function of ion energy and ion flux density. Ion energies range from 100 eV to 1000 eV. The AFM measurements are used to determine the roughness distribution across the wafers. A regular pattern of SiGe crystallites is found, where the damage due to low ion energy Si⁺-ion bombardment is medium and the degree of relaxation, determined by Raman spectroscopy, is below 25%.     

In situ observation on Au(1 0 0) surface in molten EMImBF4 by electrochemical atomic force microscopy (EC-AFM)

The Au(1 0 0) surface structure in contact with 1-ethyl-3-methylimidazolium tetrafluoroborate (EMImBF₄) has been observed using electrochemical atomic force microscopy (EC-AFM) under an electrochemically controlled potential. The AFM images, taken in EMImBF₄ in the potential range from −0.6 to 0.2 V vs. Ag/Ag(I), shows a fourfold symmetry with the distance between protrusions of ≈0.30-0.32 nm. This structure agrees well with the ideal surface structure of Au(1 0 0)-(1 × 1) and it is very similar to that previously obtained in a sulfuric acid aqueous solution.     

Enhanced surface atomic step motion observed in real time after nanoindentation of NaCl(100)

The nanometer-scale indentation of a crystalline surface produces nanostructures that evolve on a timescale that is inaccessible to existing imaging methods for the vast majority of surfaces. We have been able to observe the dynamic evolution of the freshly cleaved surface of a NaCl(100) crystal after indentation with an atomic force microscope (AFM) in air. Here we present sequential AFM images featuring vertical atomic resolution which show that atomic terrace motion is greatly enhanced by the AFM indentation. Moreover, some of the nanometric features generated by the indentation become reassimilated into the crystalline surface structure of the surroundings of the indentation over a period of time of the order of several minutes.     

The role of antiphase boundaries during ion sputtering and solid phase epitaxy of Si(0 0 1)

The Si(0 0 1) surface morphology during ion sputtering at elevated temperatures and solid phase epitaxy (SPE) following ion sputtering at room temperature has been investigated using scanning tunneling microscopy. Two types of antiphase boundaries form on Si(0 0 1) surfaces during ion sputtering and SPE. One type of antiphase boundary, the AP2 antiphase boundary, contributes to the surface roughening. AP2 antiphase boundaries are stable up to 700 °C, and ion sputtering and SPE performed at 700 °C result in atomically flat Si(0 0 1) surfaces.     

Shape variation in epitaxial microstructures of gold silicide grown on Br-passivated Si(1 1 1) surfaces

Kinetic Monte Carlo simulations for growth on substrates of three-fold symmetry predict the growth of islands of various shapes depending on the growth temperature [Phys. Rev. Lett. 71 (1993) 2967]. On Br-Si(1 1 1) substrates growth of epitaxial gold silicide islands of equilateral triangular and trapezoidal shapes have earlier been observed by annealing at the Au-Si eutectic temperature, 363 °C [Phys. Rev. B 51 (1995) 14330]. We carried out annealing with temperature variation within a small window--(363 ± 30) °C. This has led to island growth of additional shapes like regular hexagon, elongated hexagon, walled hexagon and dendrite. Some of the observed island shapes have not been predicted.     

Controlled surface nanopatterning with buried dislocation arrays

Self-assembled configurations of nanostructures are expected to play an increasing role in devices design, as an alternative to conventional microelectronics. The key limitation is the lack of control on localisation, density and size uniformity of the structures. Here we show how to create a template to overcome these problems. A periodic nanometre scale patterning can be induced at a silicon surface by buried dislocation networks obtained by twist wafer bonding, using stress selective etching of the surface. These templates are morphologically characterised by scanning tunnelling microscopy and grazing incidence X-ray diffraction. Stress fields and elastic energy densities are calculated for the non-etched solid, and the selective etching mechanisms are discussed. Germanium growth experiments on such a Si patterned surface give a demonstration of the ordering efficiency. This study provides a general method to create a template, which organises nanostructures with controlled periodicity over the full size of a Si wafer.     

Morphological evolution of SiGe layers

Extensive research activity has been devoted to self-assembly of very small coherent islands. However, while island formation is commonly described by a widely used S-K growth scheme, more complex mechanisms based on competitive effects of kinetics and thermodynamics take place during the epitaxy of Si_1−xGe_x on Si(0 0 1). The aim of this paper is to explain the formation and the evolution of Si_1−xGe_x islands on Si(0 0 1). The paper presents a comprehensive investigation of the different growth modes of Si_1−xGe_x films (with x varying from 0 to 1) on Si(0 0 1) and Si(1 1 1). The results are presented in the form of kinetic morphological growth diagrams of as-grown samples. Two and four growth regimes are distinguished on (1 1 1) and (0 0 1) respectively. These growth regimes correspond to different levels of relaxation. In particular the four regimes observed on Si(0 0 1) correspond to (i) no relaxation in regime I (2D layer), (ii) 15-20% relaxation in regime II (“huts” islands with (1 0 5) facets), (iii) 20% and 50% relaxation in regime III (in “huts” and “domes” respectively) and (iv) 50% and 80% relaxation in regime IV (“domes” with bimodal size distribution). Every growth regime characteristic of as-grown sample is also associated with a specific equilibrium steady state morphology which is obtained after long-term annealing of the as-grown samples. In the two first regimes (no or small strain relaxation) the equilibrium morphology of highly strained Si_1−xGe_x deposits corresponds to (1 0 5) faceted islands. We show that these islands are stabilised by the compressive stress. As soon as strain is released, (1 0 5) facets disappear at the expense of the (1 1 3) and (1 1 1) facets and first-order transition occurs between “huts” and “domes” islands.