Analysis of roughness of Cs surfaces via evaluation of the autocorrelation function

At low temperature prepared quench-condensed Cs surfaces are analysed on a nanometer scale via scanning tunneling microscopy. The analysis of surface roughness is presented with the help of the evaluation of their autocorrelation function. In order to extract the correct autocorrelation function we present the requirement regarding the scan resolution of scanning probe microscopy (SPM) images in general. This is supported by a ‘numerical experiment’. Furthermore, we present some methods of deducing higher orders of autocorrelation lengths, which are needed to evaluate SPM images with non-random distribution of roughness amplitudes. These characteristic values of the autocorrelation function could play the key role in further statistical calculations, e.g., on how surface roughness alters the wetting behaviour of liquid helium adsorbed on the cesium surfaces.     

Surface properties of platinum thin films as a function of plasma treatment conditions

We examined the surface properties of platinum (Pt) thin films exposed to oxygen and argon plasma treatments and compared them to as-deposited Pt films. The surface wetting properties, refractive index and extinction coefficient of the Pt films were monitored as a function of time after different plasma treatments. Surfaces treated with an oxygen plasma were dramatically different from as-deposited Pt, whereas argon plasma treated surfaces were similar to as-deposited films. X-ray photoelectron spectroscopy confirmed the formation of platinum oxide on films treated with an oxygen plasma, while such oxide diminished after argon plasma treatment. Surface morphology studied with atomic force microscopy indicated a strong dependence of the surface roughness of the Pt films on the power and duration of the argon plasma used for the treatment. Based on these studies, an oxygen plasma treatment followed by a brief low-power argon plasma etch was developed for the purpose of regenerating clean and metallic Pt surfaces, and at the same time providing the smoothest possible surface morphology.     

Overpotential deposition of Ag monolayer and bilayer on Au(1 1 1) mediated by Pb adlayer underpotential deposition/stripping cycles

Ultra-thin Ag films on the Au(1 1 1) surface were prepared via overpotential deposition (OPD) in the presence of Pb²⁺ ions. By carrying out repetitive Pb adlayer underpotential deposition (UPD) and stripping cycles during Ag bulk deposition, the two-dimensional growth of Ag films was significantly enhanced in high OPD. The Ag monolayer sample was made by comparing the voltammetry curves, in which the signatures for Pb adlayer UPD on Au(1 1 1) changed to that on Ag(1 1 1). As demonstrated by the X-ray specular reflectivity measurements, nearly complete monolayer and bilayer films can be made with optimized deposition procedures. On subatomic scale, however, we found that these films have significant higher root-mean-square displacement amplitudes than those underpotentially deposited Ag monolayer and bilayer on either Au(1 1 1) or Pt(1 1 1).     

PEEM study of work function changes in Cu, Au and Pd metal surfaces with surface acoustic wave propagation

The effects of surface acoustic wave (SAW) on the work function of Cu, Au and Pd metal surfaces with different surface structures were studied by photoelectron emission microscopy (PEEM). SAW propagation produced bright PEEM images for Cu, Au and Pd metal surfaces consisting of high-index planes and step sites, whereas it yielded dark images for the metals exposing low-index planes, indicating that the SAW enhanced photoemission from rough metal surfaces containing coordinatively-unsaturated metal atoms and lowered that from densely packed smooth metal surfaces. Changes in the PEEM images with SAW-on and SAW-off were reversible and were associated with decreases and increases in the work function of the metal surfaces, respectively. The SAW caused periodic and vertical lattice displacement, and it was demonstrated that large lattice displacement was responsible for work function changes from coincidence between the patterns of photoemission and lattice displacement. A mechanism for work function changes is proposed on the basis of effects on the spatial structures and electronic properties of metal surfaces.     

The importance of imaging conditions in scanning tunneling microscopy for the determination of surface texture and roughness

We show that the control conditions in the feedback loop of a scanning tunneling microscope (STM) affect the values of the surface texture parameters, including fractal characterization, when they are calculated from STM images of the surface. The main surface texture parameters (such as the r.m.s. roughness, kurtosis, skewness, and average wavelength) show a strong dependence on the conditions used in the feedback loop for imaging. Fractal character changes also with feedback parameters. The quality of the STM images can be measured quantitatively by using some of the surface texture parameters.     

STM and XPS characterisation of vacuum annealed nanocrystalline WO3 films

Scanning tunnelling microscopy and X-ray Photoelectron Spectroscopy were conducted on magnetron sputtered WO₃ thin films, following a sequence of ultra high vacuum anneals from 100 °C to 900 °C. Annealing from 100 °C to 400 °C induced an upward surface band bending of about 0.3 eV, attributed to the oxygen migration from the bulk to the surface, but no changes in the surface topography. Chemical changes occurred from 600 °C to 800 °C, associated with the formation of secondary oxide species. STM imaging showed that the film surface consists of amorphous particles 35 nm in size up to 600 °C, while higher temperatures resulted in an increase in particle size. Crystallisation of the nanoparticles started to occur after annealing at 600 °C. The implications in terms of gas sensing are discussed.     

Surface plasmon resonance characterization of thermally evaporated thin gold films

The heterogeneous character of thin gold films prepared by thermal evaporation and the dependence of this heterogeneity on the rate of their deposition must be considered when exploiting their optical properties for biosensor purposes. For instance, the performance of thin gold films for surface plasmon resonance (SPR) biosensors may drastically be degraded if care is not taken to prepare a film with a high fraction of gold (>95%). We use three different models to interpret the SPR response of gold films prepared by thermal evaporation. We show that the interpretation of the SPR curves requires considering both a global heterogeneity of the gold films and a surface roughness. Our conclusions are further corroborated by scanning surface plasmon microscope (SSPM) images of these thin gold films.     

Fractal analysis and atomic force microscopy measurements of surface roughness for Hastelloy C276 substrates and amorphous alumina buffer layers in coated conductors

In coated conductors, surface roughness of metallic substrates and buffer layers could significantly affect the texture of subsequently deposited buffer layers and the critical current density of superconductor layer. Atomic force microscopy (AFM) is usually utilized to measure surface roughness. However, the roughness values are actually relevant to scan scale. Fractal geometry could be exerted to analyze the scaling performance of surface roughness. In this study, four samples were prepared, which were electro polished Hastelloy C276 substrate, mechanically polished Hastelloy C276 substrate and the amorphous alumina buffer layers deposited on both the substrates by ion beam deposition. The surface roughness, described by root mean squared (RMS) and arithmetic average (R_a) values, was analyzed considering the scan scale of AFM measurements. The surfaces of amorphous alumina layers were found to be fractal in nature because of the scaling performance of roughness, while the surfaces of Hastelloy substrates were not. The flatten modification of AFM images was discussed. And the calculation of surface roughness in smaller parts divided from the whole AFM images was studied, compared with the results of actual AFM measurements of the same scan scales.     

Growth of Au thin film on Cu-modified Si(1 1 1) surface

Miniaturizing of electronic devices requires that conductive elements maintain advanced electrical characteristics upon reducing their geometrical sizes. For gold, which is valued for its high electrical conductivity and stability against ambient conditions, creation of extra-thin films on silicon is hampered by formation of the quite complex Au/Si interface. In the present work, by forming a Si(1 1 1)5.55 × 5.55-Cu surface reconstruction prior to Au deposition we formed Au films with smoother surface morphology and higher surface conductivity compared to Au film grown on a pristine Si(1 1 1)7 × 7 surface. Scanning tunnelling microscopy and four-point probe measurements were used to characterize the growth mode of the Au film on a Si(1 1 1)5.55 × 5.55-Cu reconstruction at room temperature.     

Mass and lattice effects in trapping: Ar, Kr, and Xe on Pt(1 1 1), Pd(1 1 1), and Ni(1 1 1)

The trapping probabilities of argon, krypton, and xenon on Pd(1 1 1) and Ni(1 1 1) have been investigated using supersonic molecular beam techniques. The trapping probability of argon exhibits normal incident energy in a similar fashion on both Pd(1 1 1) and Pt(1 1 1) because the mass of argon is significantly less than the surface mass of either Pd or Pt. In contrast, dynamic corrugation in the gas-surface potential is observed for krypton trapping on Pt(1 1 1) and Pd(1 1 1), resulting in a decreased angular dependence of the trapping probability compared to argon. For xenon trapping on Pd significant lattice deformation during the gas-surface collision appears to give rise to total energy scaling. The trapping probability of xenon on Pd(1 1 1) remains high at unusually high incident kinetic energies due to the overall enhanced energy transfer from the incident atom to the lattice. Trapping probabilities of Ar, Kr, and Xe are significantly lower on Ni(1 1 1) than on either Pt(1 1 1) or Pd(1 1 1) despite the lower surface mass of the Ni atoms. This result is attributed to the lower binding energy of the rare gases on Ni(1 1 1) and the higher Debye temperature of Ni. The energy scaling of Ar trapping on Ni(1 1 1) is determined by static corrugation, but the energy scaling for Kr and Xe on Ni(1 1 1) may involve the effects of dynamic corrugation. In the latter cases, the greater stiffness of the nickel lattice decreases the dynamic corrugation relative to Pt(1 1 1) and Pd(1 1 1).     

A computer program for automated step edge motion analysis from scanning probe microscopy images

A computer algorithm was developed to automatically track the displacement of straight step edges between sequential scanning probe microscopy images of single-crystal surfaces. The program utilizes the Canny edge detection algorithm followed by the Hough Transform of the edge map to identify step edges according to their direction, relative to the image axes, and according to their displacement, relative to the image origin. The tracking of individual steps is facilitated by the fact that straight edges in general maintain their direction and therefore, steps of similar displacement but different direction can be sorted. The algorithm is based on the assumption that the rate of image acquisition is much greater than the rate of (mono)layer growth/dissolution, requiring that changes in step displacement are small in successive images. The change in step displacement in sequential images leads directly to the calculation of the step speed. By tabulating all changes in step displacement through a sequence of images, a statistical representation of the step edge data is produced. The program was evaluated using a sequence of 20 atomic force microscopy images from a calcite (104) surface growing from a supersaturated aqueous solution. The program required, in total, 5 CPU-minutes running on a Pentium 4 processor to compute the mean step speed with 60% precision whereas the equivalent number of measurements performed “by hand” required 6 person-hours at 70% precision. For comparable output, the computer program therefore represents a factor of about 100 decrease in required effort.     

Spatio-temporal dynamics of the NO + NH3 reaction on polycrystalline platinum

Spontaneous reaction rate oscillations and spatio-temporal patterns have been observed by mass spectrometry and photoemission electron microscopy (PEEM) during the reduction of NO by NH₃ on polycrystalline platinum at 1 × 10⁻⁴ Torr and temperatures from 460-520 K. The appearance of both oscillations and patterns was found to be strongly dependent on the gas phase composition and the temperature. In addition, the overall dynamics of the catalyst were found to be dominated by the nonlinear behavior of Pt(1 0 0) type grains, while other types of grains did not participate. In contrast to previous studies, a large number of complex multimodal oscillations were observed, particularly as the coupling between the surface and the gas phase was increased. The appearance of these complex oscillations demonstrates the importance of gas phase coupling to understanding catalytic reactions, even in high vacuum systems.     

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.     

Revisiting the physical processes of vapodeposited thin gold films on chemically modified glass by atomic force and surface plasmon microscopies

The preparation of very thin (at the scale of a few tens of nanometers) gold films by thermal evaporation and deposition on a solid substrate (glass) remains a key step for the elaboration of transparent and sensitive optical biosensors. We study the influence of the glass surface treatment and its thermal conductivity on the structure and composition of evaporated gold films. Using a combination of atomic force microscopy (AFM), high resolution surface plasmon resonance (SPR) imaging, and X-ray photoelectron spectroscopy (XPS), we demonstrate that the grafting of a layer of long chain mercaptant, using 11-mercaptoundecyltrimethoxysilane (S_ξSi), prior to gold deposition produces a drastic modification of gold inner and surface textures. A thorough investigation of AFM image topography by 2D wavelet-based segmentation method reveals the flat conical shape of the gold surface grains and their shape invariance with the glass surface chemical treatment. However, this treatment leads to a drastic decrease of the mean size and polydispersity of these grains by a factor of 2, thereby lowering the gold surface roughness. The rationale is that the combination of surface forces and thermal transfer drives the formation of homogeneous and flatter gold films.     

Optical properties of gold electrode surfaces covered with metal monolayers

The relative reflectivity changes ΔR/R of a gold electrode surface caused by the deposition of monolayers of thallium, copper and lead from electrolytic solutions at underpotentials have been studied in situ in the photon energy range between 1.8 and 5.2 eV. The optical constants of the surface layer giving rise to this measured reflectivity change have been calculated and compared to the results of the electroreflectance effect on bare gold surfaces. It is shown that the reflectance change observed during the monolayer deposition is to first order due to a change in the gold electrode surface layer and not to absorption processes in the monolayer itself. The latter ones cause a fine structure superimposed to the substrate spectrum. The relatively strong change in the gold surface optical constants upon metal monolayer deposition is explained in terms of an enhanced electroreflectance effect due to the partially ionic character of the metal adatoms, which alters the free electron concentration in the substrate surface layer. Electroreflectance spectra obtained on gold surfaces covered with a monolayer of thallium compare favourably with dielectric loss functions computed for charged gold surfaces. This supports the assumption that the reflectivity changes observed upon metal monolayer deposition are mostly due to changes in the optical properties of the substrate metal surface.     

Vicinal and on-axis surfaces of 6H-SiC(0001) thin films observed by scanning tunneling microscopy

Surfaces of 6H-SiC(0001) homoepitaxial layers deposited on vicinal (3.5° off (0001) towards [11 0]) and on-axis 6H---SiC wafers by chemical vapour deposition have been investigated using ultra-high vacuum scanning tunneling microscopy. Undulating step configurations were observed on both the on-axis and the vicinal surfaces. The former surface possessed wider terraces than the latter. Step heights on both surfaces were 0.25 nm corresponding to single bilayers containing one Si and one C layer. After annealing at T>1100°C for 3–5 min in UHV, selected terraces contained honeycomb-like regions caused by the transformation to a graphitic surface as a result of Si sublimation. A model of the observed step configuration has been proposed based on the observation of the [ 110] or [1 10] orientations of the steps and energetic considerations. Additional deposition of very thin (2 nm) SiC films on the above samples by gas source molecular beam epitaxy was performed to observe the evolution of the surface structure. Step bunching and growth of 6H---SiC layers and formation of 3C---SiC islands were observed on the vicinal and the on-axis surfaces, respectively, and controlled by the diffusion lengths of the adatoms.     

Electron spectroscopy studies of surface In-Ag alloy formation on the tungsten surface

XPS and UPS investigations of ultrathin films of In/Ag and Ag/In, deposited onto the W(1 1 0) surface in the ultrahigh vacuum conditions have been performed. Indium and silver films were formed by “in-situ” evaporation on W(1 1 0) substrate. XPS and UPS studies have been performed by means of SCIENTA ESCA200 instrument. The changes of In4d core-level and Ag4d valence band emissions with increasing Ag and In coverage were monitored to observe the energy shift and shape of the spin-orbit doublet of In4d and Ag4d lines in the Ag/In/W and In/Ag/W systems. UPS (HeI and HeII) measurements were supported by XPS AlK_α measurements of In3d and W4p levels, as well as by investigations of Ag3d levels. XPS and UPS data allowed to evaluate the coverage and make conclusions concerning intermixing and surface alloying in the In/Ag/W and Ag/In/W systems. W(1 1 0) substrate can be cleaned after each deposition by thermal desorption and no alloying in the In/W and Ag/W systems is observed.     

Gold coated metal nanostructures grown by glancing angle deposition and pulsed electroplating

Nickel based nanostructures are grown by glancing angle deposition (GLAD) on flat and pre-patterned substrates. These fabricated porous thin films were subsequently coated by pulsed electroplating with gold. The morphology and conformity of the gold coating were investigated by scanning electron microscopy and X-ray diffraction. Controlled growth of closed gold layers on the nanostructures could be achieved, while the open-pore structure of the nanosculptured thin films was preserved. Such gold coated nanostructures are a candidate for optical sensing and catalysis applications. The demonstrated method can be applied for numerous material combinations, allowing to provide GLAD thin films with new surface properties.     

Properties of the roughness in NiFe/FeMn exchange-biased system

X-ray reflectivity and atomic force microscopy analyses were performed in the Si/WTi (7 nm)/NiFe (5 nm)/FeMn (13 nm)/WTi (7 nm) exchange-biased system prepared by magnetron sputtering. Layer-by-layer analyses were done in order to have interfacial roughness parameters quantitatively. X-ray reflectivity results indicate that the successive layer deposition gives rise to a cumulative roughness. In addition, the atomic force microscopic images analyses have revealed that the roughness enhancement caused by the successive layer deposition can be associated with an appearance of a longer wavelength roughness induced by the NiFe layer deposition.