Influence of atomic force microscopy acquisition parameters on thin film roughness analysis

A reliable procedure for measuring parameters connected to surface roughness is needed to compare the gas sensing properties of various thin films or the effect of different fabrication procedures on the surface roughness and the sensing properties. In this article, we propose to investigate how the acquisition parameters specific to atomic force microscopy investigations such as pixel size, scan area and scan speed influence the roughness parameters, namely root mean square and surface area ratio, commonly used for characterizing the gas sensing properties of porphyrins and other materials.     

Surface roughness and filler particles characterization of resin‐based composites

The purpose of this study was to evaluate the surface roughness (Ra), and the morphology and composition of filler particles of different composites submitted to toothbrushing and water storage. Disc‐shaped specimens (15 mm × 2 mm) were made from five composites: two conventional (Z100?, and Filtek? Supreme Ultra Universal, 3M), one “quick‐cure” (Estelite ∑ Quick, Tokuyama), one fluoride‐releasing (Beautiful II, Shofu), and one self‐adhering (Vertise Flow, Kerr) composite. Samples were finished/polished using aluminum oxide discs (Sof‐Lex, 3M), and their surfaces were analyzed by profilometry (n = 5) and scanning electron microscopy (SEM; n = 3) at 1 week and after 30,000 toothbrushing cycles and 6‐month water storage. Ra data were analyzed by two‐way analysis of variance and Tukey's test (α = 0.05). Filler particles morphology and composition were analyzed by SEM and X‐ray dispersive energy spectroscopy, respectively. Finishing/polishing resulted in similar Ra for all the composites, while toothbrushing and water storage increased the Ra of all the tested materials, also changing their surface morphology. Beautifil II and Vertise Flow presented the highest Ra after toothbrushing and water storage. Filler particles were mainly composed of silicon, zirconium, aluminum, barium, and ytterbium. Size and morphology of fillers, and composition of the tested composites influenced their Ra when samples were submitted to toothbrushing and water storage.     

Spin‐coated epoxy resin embedding technique enables facile SEM/FIB thickness determination of porous metal oxide ultra‐thin films

A facile nonsubjective method was designed to measure porous nonconductive iron oxide film thickness using a combination of a focused ion beam (FIB) and scanning electron microscopy. Iron oxide films are inherently nonconductive and porous, therefore the objective of this investigation was to optimize a methodology that would increase the conductivity of the film to facilitate high resolution imaging with a scanning electron microscopy and to preserve the porous nature of the film that could potentially be damaged by the energy of the FIB. Sputter coating the sample with a thin layer of iridium before creating the cross section with the FIB decreased sample charging and drifting, but differentiating the iron layer from the iridium coating with backscattered electron imaging was not definitive, making accurate assumptions of the delineation between the two metals difficult. Moreover, the porous nature of the film was lost due to beam damage following the FIB process. A thin layer plastication technique was therefore used to embed the porous film in epoxy resin that would provide support for the film during the FIB process. However, the thickness of the resin created using conventional thin layer plastication processing varied across the sample, making the measuring process only possible in areas where the resin layer was at its thinnest. Such variation required navigating the area for ideal milling areas, which increased the subjectivity of the process. We present a method to create uniform thin resin layers, of controlled thickness, that are ideal for quantifying the thickness of porous nonconductive films with FIB/scanning electron microscopy.     

Antimicrobial effect,frictional resistance,and surface roughness of stainless steel orthodontic brackets coated with nanofilms of silver and titanium oxide: a preliminary study

Nano‐silver and nano‐titanium oxide films can be coated over brackets in order to reduce bacterial aggregation and friction. However, their antimicrobial efficacy, surface roughness, and frictional resistance are not assessed before. Fifty‐five stainless‐steel brackets were divided into 5 groups of 11 brackets each: uncoated brackets, brackets coated with 60 µm silver, 100 µm silver, 60 µm titanium, and 100 µm titanium. Coating was performed using physical vapor deposition method. For friction test, three brackets from each group were randomly selected and tested. For scanning electron microscopy and atomic‐force microscopy assessments, one and one brackets were selected from each group. For antibacterial assessment, six brackets were selected from each group. Of them, three were immediately subjected to direct contact with S. mutans. Colonies were counted 3, 6, 24, and 48 h of contact. The other three were stored in water for 3 months. Then were subjected to a similar direct contact test. Results pertaining to both subgroups were combined. Groups were compared statistically. Mean (SD) friction values of the groups 'control, silver‐60, silver‐100, titanium‐60, and titanium‐100' were 0.55 ± 0.14, 0.77 ± 0.08, 0.82 ± 0.11, 1.52 ± 0.24, and 1.57 ± 0.41 N, respectively (p = .0004, Kruskal–Wallis). Titanium frictions were significantly greater than control (p < .05), but silver groups were not (p > .05, Dunn). In the uncoated group, colony count increased exponentially within 48 h. The coated groups showed significant reductions in colony count (p < .05, two‐way‐repeated‐measures ANOVA). In conclusions, all four explained coatings reduce surface roughness and bacterial growth. Nano‐titanium films are not suitable for friction reduction. Nano‐silver results were not conclusive and need future larger studies.     

Assessing conformal thin film growth under nonstochastic deposition conditions: application of a phenomenological model of roughness replication to synthetic topographic images

In this work, a simple method to follow the evolution of the surface of thin films during growth on substrates characterised by high roughness is detailed. To account for real cases as much as possible, the approach presented is based on the hypothesis that deposition takes place under nonstochastic conditions, such as those typical of many thin film processes in industry and technology. In this context, previous models for roughness replication, which are mainly based on idealised deposition conditions, cannot be applied and thus ad hoc approaches are required for achieving quantitative predictions. Here it is suggested that under nonstochastic conditions a phenomenological relation can be proposed, mainly based on local roughening of surface, to monitor the statistical similarity between the film and the substrate during growth or, in other words, to detect changes of the bare substrate morphological profile occurring during the film growth on top. Such approximation is based on surface representation in terms of power spectral density of surface heights, derived from topographic images; in this work, such method will be tested on two separate batches of synthetic images which simulate thin films growth onto a real rough substrate. In particular, two growth models will be implemented: the first reproduces the surface profile obtained during an atomic force microscopy measurement by using a simple geometrical envelope of surface, regardless the thin film growth mechanism; the second reproduces the columnar growth expected under nonstochastic deposition conditions. It will be shown that the approach introduced is capable to highlight differences between the two batches and, in the second case, to quantitatively account for the replication of the substrate roughness during growth. The results obtained here are potentially interesting in that they account essentially for the geometrical features of the surfaces, and as such they can be applied to synthetic depositions that reproduce different thin film depositions and experimental contexts.     

Surface roughness measurements as a method for tribological characterisation of ball bearings

A series of experiments using steel or hybrid balls in an SNFA VEX25 type bearing was conducted, at a rotational speed of 50,000 rpm. The race material was 100Cr6 steel, whereas for the balls various steels, coatings, and ceramics were used. The different materials used for the balls as well as the method of lubrication (air/oil or grease) strongly influenced the surface degradation of the ball bearings. Hybrid bearings with ceramic balls showed very little wear of either the balls or the steel races, and so offer potential for high‐speed applications. The degradation of the bearings was examined using scanning electron microscopy, atomic force microscopy, and laser scanning profilometry. The disadvantages and advantages of these methods are given, along with the results of surface roughness measurements.     

Investigation of mercury adsorption on gold films by STM

Scanning tunnelling microscopy, combined with complementary electrical and analytical measurements, provides a powerful method for examining the behaviour of mercury on gold-film sensors under actual sensor operating conditions. The films exhibit a linear increase in resistance upon adsorption of mercury, and this resistive change is accompanied by a decrease in measured barrier height at submonolayer coverages of mercury. STM studies of changes in the effective barrier height upon mercury adsorption provide evidence that mercury migrates to grain boundaries for films exposed at submonolayer coverages. Coverages in excess of a monolayer result in a nearly constant, reduced effective barrier height across the entire surface, which is indicative of a more uniform distribution of mercury over the surface. This behaviour is interpreted in terms of the adsorption of mercury onto defective, contaminated gold surfaces.     

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.     

Microstructure and interfacial chemistry of pure and La‐doped BiFeO3 thin films

We report on the microstructure and interfacial chemistry of thin films of pure and La‐doped multiferroic bismuth ferrite (Bi_1‐xLa_xFeO₃ or BLFO), synthesized on Indium Tin Oxide‐coated glass substrates by solution‐deposition technique and studied using scanning transmission electron microscopy. Our results show that undoped and La‐doped thin films are polycrystalline with distorted rhombohedral structure without any presence of any line or planar defect in the films. In addition, the films with La doping did not show any structural change and maintain the equilibrium structure. Cross section compositional analysis using X‐ray energy dispersive spectrometry did not reveal either any interdiffusion of chemical species or formation of reaction product at the film‐substrate interface. However, a closer examination of the microstructure of the films shows tiny pores along with the presence of ～2–3 nm thin amorphous layers, which may have significant influence on the functional properties of such films. Microsc. Res. Tech. 76:1304–1309, 2013. © 2013 Wiley Periodicals, Inc.     

A scanning conduction microscopic method for probing abrasion of insulating thin films

The use of scanning force microscopy (SFM) to probe wear processes at interfaces is of considerable interest. We present here a simple modification of the SFM which allows us to make highly spatially resolved measurements of conductivity changes produced by abrasion of thin insulating films on metal substrates. The technique is demonstrated on fluorocarbon polymer thin films deposited on stainless steel substrates.     

Fractal features of carbon–nickel composite thin films

This work analyses the three‐dimensional (3‐D) surface texture of carbon–nickel (C–Ni) films grown by radio frequency (RF) magnetron co‐sputtering on glass substrates. The C–Ni thin films were deposited under different deposition times, from 50 to 600 s, at room temperature. Atomic force microscopy was employed to characterize the 3‐D surface texture data in connection with the statistical, and fractal analyses. It has been found that up to 180 s the sputtering occurs in more metal content mode and in greater than 180 s it occurs in more non‐metal content mode. This behavior demonstrated a strong link between the structural and morphological properties of C–Ni composite films and facilitates a deeper understanding of structure/property relationships and surface defects in prepared samples. Furthermore, these findings can be applied to research on the mechanisms to prepare and control high‐quality C–Ni films.     

Nanotribology: an UHV-SFM study on thin films of AgBr(001)

We performed scanning force microscopy (SFM) in ultrahigh vacuum (UHV) on AgBr thin films which were in situ deposited on NaCl(001) substrates. The morphology of the initial growth stage and the nanotribological properties of these thin films are characterized and discussed. The lateral (frictional) forces are measured as a function of normal load. The local friction coefficients are extracted by means of the two-dimensional histogram technique. In the low load regime, friction coefficients of 0.33 ± 0.07 and <0.03 are found between probing SiO _x tip and AgBr and NaCl, respectively. The two-dimensional histogram reveals the transition from the force regime of wearless friction to the initial stage of wear on this thin film system. High-resolution SFM images of AgBr(001) are presented which reveal the atomic-scale periodicity of an unreconstructed AgBr(001) surface. The stick-slip nature of the frictional force is demonstrated.     

SEM and AFM studies of dip‐coated CuO nanofilms

Cupric oxide (CuO) semiconducting thin films were prepared at various copper sulfate concentrations by dip coating. The copper sulfate concentration was varied to yield films of thicknesses in the range of 445–685 nm by surface profilometer. X‐ray diffraction patterns revealed that the deposited films were polycrystalline in nature with monoclinic structure of (?111) plane. The surface morphology and topography of monoclinic‐phase CuO thin films were examined using scanning electron microscopy (SEM) and atomic force microscopy (AFM), respectively. Surface roughness profile was plotted using WSxM software and the estimated surface roughness was about ～19.4 nm at 30 mM molar concentration. The nanosheets shaped grains were observed by SEM and AFM studies. The stoichiometric compound formation was observed at 30 mM copper sulfate concentration prepared film by EDX. The indirect band gap energy of CuO films was increased from 1.08 to 1.20 eV with the increase of copper sulfate concentrations. Microsc. Res. Tech., 2013. © 2012 Wiley Periodicals, Inc.     

Influence of gallium‐doped zinc‐oxide thickness on polymer light‐emitting diode luminescence efficiency

Conducting atomic force microscopy and scanning surface potential microscopy were used to study the local electrical properties of gallium‐doped zinc oxide (GZO) films prepared by pulsed laser deposition (PLD) on a polyimide (PI) substrate. For a PLD deposition process time of 8 min, the root‐mean‐square roughness, coverage percentage of the conducting regions, and mean work function on the GZO surface were 2.33 nm, 96.6%, and 4.82 eV, respectively. When the GZO/PI substrate was used for a polymer light‐emitting diode (PLED), the electroluminescence intensity increased by nearly 20% compared to a standard PLED, which was based on a commercial‐ITO/glass substrate. Microsc. Res. Tech. 76:783–787, 2013. © 2013 Wiley Periodicals, Inc.     

Influence of surface roughness features on mixed‐film lubrication

An optical technique (three‐dimensional spacer layer imaging) has been developed to map accurately lubricant film thickness in thin‐film elastohydrodynamic (EHD) contacts. This experimental technique has been used to study the influence of surface roughness features, asperity height, and slope on EHD film thickness and pressure. Single ridges transverse to the entrainment direction were used to represent asperities. It was found that the ridges with lower slopes generate films of greater minimum thickness. Below a certain entrainment speed, the minimum film thickness declined at a rate dependent on the ridge slope. At low speeds, the ridges with higher slopes entrapped a larger volume of lubricant ahead of the ridge and along the entrainment direction. For all speeds, the highest ridges entrapped the most lubricant. Both ridge slope and ridge height had a negligible effect on mean film thickness in the contact. Asperity pressure increased with higher ridge slope, but was not influenced by entrainment speed. An increase in pressure was found where lubricant is entrapped upstream of a ridge.     

Structure analysis of sputter-coated and ion-beam sputter-coated films: a comparative study

Gold, platinum and tungsten films were deposited by low energy input (7 mA, 450 V), or high deposition rate (80 mA, 1500 V), diode sputter coating and by ion beam sputter coating. Film structures on Formvar coated grids and on the surface of coated erythrocytes, resin embedded, sectioned, and recorded at high magnification in a TEM were compared using computer-assisted measurements and analysis of film thickness and grain size. The average grain size of the thinnest gold and platinum films was relatively independent of the mode or rate of deposition but as the film thickness increased, significant differences in grain size and film structure were observed. Thick platinum or gold films deposited by low energy input sputter coating contained large grain size and electron transparent cracks; however, more even films with narrower cracks but larger grain size were produced at high deposition rates. Ion beam sputter coated gold had relatively large grain size in 10 nm thick films, but beyond this thickness the grains coalesced to form a continuous film. Platinum films deposited by ion beam sputter coating were even and free of electron transparent cracks and had a very small grain size (1–2 nm), which was relatively independent of the film thickness. Tungsten deposition either by low energy input or ion beam sputter coating resulted in fine grained even films which were free of electron transparent cracks. Such films remained granular in substructure and had a grain size of about 1 nm which was relatively independent of film thickness. Tungsten films produced at high deposition rates were of poorer quality. We conclude that thick diode sputter coated platinum and gold films are best deposited at high deposition rates provided the specimens are not heat sensitive, the improvement in film structure being more significant than the slight increase in grain size. Thick diode or ion beam sputter coated gold films should be suitable for low resolution SEM, and thin discontinuous gold films for medium resolution SEM. Diode sputter coated platinum should be suitable for medium resolution SEM and ion beam sputter coated platinum for medium and some high resolution SEM. 1–5 nm thick tungsten films, deposited by low energy input or ion beam sputter coating should be suitable for high resolution SEM, particularly where contrast is of less importance than resolution.     

Nucleation and growth of Cu and Ag on Si(111)7×7

By using scanning tunnelling microscopy and spectroscopy we have studied condensation of Cu and Ag on Si(111)7×7 between room temperature and 130°C in the submonolayer and monolayer range. For submonolayer coverage, both metals develop regular clusters on top of the inner adatoms of 7×7 unit cell halves, which we assign to the initial nuclei of metal condensation. The metal film growth continues by adding further metal atoms to these clusters until one half of the 7×7 unit cell is covered completely with a triangular 2-D metal island. For a coverage of three monolayers neither Cu nor Ag grows in a layer-by-layer mode. Characteristic differences observed for both metals may be explained by the more reactive nature of Cu.     

Surface characterization and monitoring of surface changes after conservation treatments of silver gelatin photographic papers using confocal microscopy

Surface metrology techniques that are non‐perturbing (non‐contact, non‐invasive, and non‐destructive) are well suited to in situ surface studies of historical and fine art photographs. They allow for the quantitative examination of the microstructure of the photograph surface, thereby, offering an important advancement in the examination, documentation, and characterization of silver gelatin photographs and other modern and/or historic imaging materials. This article presents the application of an optical confocal scanning disk microscopy system to the qualitative and quantitative characterization and assessment of a silver gelatin photographic paper, Ilford Glossy, submitted to different humidification and flattening protocols. SCANNING 32: 122–133, 2010. © 2010 Wiley Periodicals, Inc.     

Microtribological behaviour of thin DLC films using different testing methods

To enhance the lifetime and reliability of microcomponents, thin microtribological films are applied to microparts. With reduction of the component size, investigation methods for tribological testing must be adapted. This paper studies the microtribological behaviour of thin diamond‐like carbon (DLC) films using different testing methods. To tie in with macroscopic results, to determine friction we used the well‐known pin‐on‐disc test with spherical surfaces of 10 mm diameter under a typical load of 3 N. For investigations of the behaviour under single asperity contact, Atomic Force Microscope (AFM) methods with applied loads of a few hundred micronewtons were used. Investigations on thin DLC films showed that the friction coefficient under single asperity contact is strongly dependent on the applied load and the resulting contact area. Especially for thin films (up to a few hundred nanometres) the friction coefficient is influenced by the substrate material. With decreasing substrate Young's modulus the friction coefficient also decreases. On the other hand, an increase in the abrasive wear resistance was observed using soft substrate materials. In this paper we show that the friction coefficient was also reduced by a simple surface structure. For investigations we used photolithography to create concentric circles in different substrates. This resulted in a behaviour like riding on rails for the pin‐on‐disc test. Depending on the tribological pairing the friction coefficient was reduced to more than 50% of the original value. Copyright © 2006 John Wiley & Sons, Ltd.