Morphology of Co–Cr–Mo dental alloy surfaces polished by three different mechanical procedures

The present study aims at characterizing the three‐dimensional (3‐D) morphology of a Co–Cr–Mo dental alloy surface as a result of three different procedures used for polishing it. The sample surface morphology of the sampled surface was examined employing atomic force microscopy (AFM), statistical surface roughness parameters, and fractal analysis. An extra‐hard dental alloy of cobalt–chromium–molybdenum (Co–Cr–Mo) (Wironit^®, from BEGO, Bremen, Germany) was prepared and moulded. Different polishing treatments were carried out on three groups of six samples each—a total of 18 samples. The first group contained six electropolished (EP) samples. The second group containing six samples went through a mechanical polishing process employing green rubber discs and a high shine polishing paste applied by a rotating black brush (BB). The third group comprising six samples as well went through a mechanical polishing process by means of green rubber discs, high shine polishing paste, and a rotating deer leather brush (DL). Fractal analysis on the basis of a computational algorithm applied to the AFM data was employed for the 3‐D quantitative characterization of the morphology of the sampled surfaces. The fractal dimension D (average ± standard deviation) of 3‐D surfaces for BB samples (2.19 ± 0.07) is lower than that of the DL samples (2.24 ± 0.08), which is still lower than that of the EP samples (2.27 ± 0.09). The results indicated the BB samples as presenting the lowest values of statistical surface roughness parameters, thus the best surface finish, while the EP samples yielded the highest values. Microsc. Res. Tech. 78:831–839, 2015. © 2015 Wiley Periodicals, Inc.     

Micromorphological characterization of zinc/silver particle composite coatings

The aim of this study was to evaluate the three‐dimensional (3D) surface micromorphology of zinc/silver particles (Zn/AgPs) composite coatings with antibacterial activity prepared using an electrodeposition technique. These 3D nanostructures were investigated over square areas of 5 μm × 5 μm by atomic force microscopy (AFM), fractal, and wavelet analysis. The fractal analysis of 3D surface roughness revealed that (Zn/AgPs) composite coatings have fractal geometry. Triangulation method, based on the linear interpolation type, applied for AFM data was employed in order to characterise the surfaces topographically (in amplitude, spatial distribution and pattern of surface characteristics). The surface fractal dimension D_f, as well as height values distribution have been determined for the 3D nanostructure surfaces. Microsc. Res. Tech. 78:1082–1089, 2015. © 2015 The Authors published by Wiley Periodicals, Inc.     

Influence of the artificial saliva storage on 3‐D surface texture characteristics of contemporary dental nanocomposites

The aim of this study was to analyse the influence of the artificial saliva on a three‐dimensional (3‐D) surface texture of contemporary dental composites. The representatives of four composites types were tested: nanofilled (Filtek Ultimate Body, FUB), nanohybrid (Filtek Z550, FZ550), microfilled (Gradia Direct, GD) and microhybrid (Filtek Z250, FZ250). The specimens were polymerised and polished by the multistep protocol (SuperSnap, Shofu). Their surface was examined, before and after 3 weeks’ exposure to artificial saliva storage. The surface texture was analysed using the atomic force microscope (AFM). The obtained images were processed to calculate the areal autocorrelation function (AACF), anisotropy ratio S_tr (texture aspect ratio), and structure function (SF). The log–log plots of SF were used to calculate fractal properties, such as fractal dimension D, and pseudo‐topothesy K. The analysis showed changes in surface anisotropy ratio S_tr values, which became higher, whereas the S_q roughness (root‐mean‐square) reduced after the artificial saliva storage. All the samples exhibited bifractal structure before the saliva treatment, but only half of them remained bifractal afterwards (GD, FZ250), whereas the other half turned into a monofractal (FUB, FZ550). The cube‐count fractal dimension D_cc was found to be material‐ and treatment‐insensitive.     

Two‐ and three‐dimensional profilometer assessments to determine titanium roughness

In this study, a comparative topography analysis of titanium (Ti) surfaces was performed using two‐ (2D) and three‐dimensional (3D) profilometers. Ti samples were either only sandblasted (SB) using Al₂O₃ particles or were SB and received an additional chemical treatment using a solution of 4% HF (SLA). Samples with no treatment were used as a control group (C). Therefore, three different surfaces were evaluated: SB, SLA and C. The Ti surface topographies were evaluated by scanning electron microscopy. An Ra roughness measurement was performed on each Ti sample by 2D and 3D profilometers. Surface roughness was also characterized using amplitude, spatial and hybrid 3D parameters. 2D and 3D profilometer analyses produced very close results. Mean Ra values range from 0.19 to 0.25 (C, p<0.05), 0.84 to 0.99 (SLA, p<0.05) and 0.98 to 1 µm (SB, p>0.05). The statistically different Ra values depending on the surface studied may be explained by methodological and technical differences. Also, 3D profilometer seems to be the more appropriate analytical method for measuring the roughness of Ti surfaces because it also describes surface organization. SCANNING 31: 174–179, 2009. © 2009 Wiley Periodicals, Inc.     

3D and 2D structural characterization of 1D Al/Al2O3 biphasic nanostructures

1D Al/Al₂O₃ nanostructures have been synthesized by chemical vapour deposition (CVD) of the molecular precursor [^tBuOAlH₂]₂. The deposited nanostructures grow chaotically on the substrate forming a layer with a high porosity (80%). Depending on the deposition time, diverse nanostructured surfaces with different distribution densities were achieved. A three‐dimensional (3D) reconstruction has been evaluated for every nanostructure density using the Focus Ion Beam (FIB) tomography technique and reconstruction software tools. Several structural parameters such as porosity, Euler number, geometrical tortuosity and aspect ratio have been quantified through the analysis with specified software of the reconstructions. Additionally roughness of the prepared surfaces has been characterized at micro‐ and nanoscale using profilometry and AFM techniques, respectively. While high aspects ratio around 20–30 indicates a strong anisotropy in the structure, high porosity values (around 80%) is observed as a consequence of highly tangled geometry of such 1D nanostructures.     

The effect of surface treatments on the microroughness of laser-sintered and vacuum-cast base metal alloys for dental prosthetic frameworks

This study aimed to evaluate the effect of four chemomechanical surface treatments on the surface average microroughness and profile of laser‐sintered and vacuum‐cast dental prosthetic structures. Square‐shaped blocks (10 mm × 10 mm × 1.5 mm) were prepared as follows: (1) laser‐sintered Co? Cr (L) (ST2724G); (2) cast Co? Cr (C) (Gemium‐cn); and (3) cast Ni? Cr? Ti (T) (Tilite). Specimens of each alloy group were randomly divided into five subgroups (n = 10 each), depending on the conditioning method used: (1) no treatment (control); (2) sandblasting (125 μm Al₂O₃‐particles); (3) silica coating (50 μm silica‐modified Al₂O₃‐particles); (4) oxidation; and (5) oxidation plus opacification. Subgroups 2 and 3 represent “inner” pretreatments proposed for ceramometal restorations to improve the metal surface area available for luting cements. Subgroups 4 and 5 are the “outer” pretreatments required for bonding the aesthetic veneering ceramics to the underlying metal frameworks. Average surface roughness (Ra/μm) was determined using a surface profilometer. Data were analyzed by two‐way ANOVA and Student–Newman–Keuls tests (α = 0.05). Metal surface topography was SEM‐analyzed. Despite the inner pretreatment applied, L samples resulted in the highest microroughness (P < 0.001), whereas sandblasting produced a surface‐smoothing effect in cast specimens. After oxidation, a significant increase in surface roughness occurred in all groups compared with controls, L specimens being the roughest (P < 0.001). Opacification caused a flattening effect of all oxidized structures; all opacified groups resulting in similar microroughness. Laser sintering of Co? Cr enhances the roughness of metal structures, which may improve the frameworks' microretention of the cements, and of the opaquer before the copings are veneered with the aesthetic ceramics. Microsc. Res. Tech. 75:1206–1212, 2012. © 2012 Wiley Periodicals, Inc.     

The effects of deposition time on the nanoscale patterns of Ag/DLC nanocomposite synthesized by RF‐PECVD

Introduction: In this study, a stereometric analysis of the three dimensional (3‐D) surfaces of the Ag/DLC nanocomposite synthesized by RF‐PECVD was performed. Materials and methods: Atomic force microscopy in noncontact mode was used to study surface morphology in correlation with multi‐parametric statistical analysis. The associated parameters of segmented motifs in conformity with ISO 25178‐2:, 2012 have been extracted using MountainsMap® Premium software. The mathematical algorithm computes detached watersheds of hill or dale motifs and determines the maximum and minimum points of motifs. Results and discussion: The stereometric analyses with MountainsMap® Premium software provided detailed information on the 3‐D surface topography of samples. Fractal analyses revealed the fractal nature of the performed samples is in correlation with the deposition time of samples. Detailed information of manufactured Ag/diamond‐like carbon (DLC) nanocomposite is given based on the information about the surface structure, properties, and performance characteristics. The performed analysis allows the high‐resolution modeling of Ag/DLC nanocomposite surface microtexture with motif analysis (intrinsic characteristics disclosure and characterization of surfaces fractal), in order to be included in computer interactive simulation algorithms. Conclusion: It was found the fractal dimension decreases with the increase of the deposition times on samples.     

Atomic force microscopy and energy dispersive X‐ray spectrophotometry analysis of reciprocating and continuous rotary nickel‐titanium instruments following root canal retreatment

The aim was to examine the effect of retreatment process on the surface roughness and nickel titanium (NiTi) composition of ProTaper Universal Retreatment (PTUR; consists of 3 files; D1, D2, D3) and WaveOne Gold (WOG) (primary) instruments. Twenty extracted mandibular molar teeth with severe curved (30–40°) mesial roots were selected and divided into two groups (n = 10) based on the instrument used for the removal of the root canal filling. Before and after using the instruments in two canals, they were subjected to atomic force microscopy (AFM) and energy dispersive X‐ray spectrophotometry (EDX) analysis. The EDX analysis data and roughness average (Ra) and root mean square (RMS) values were analyzed statistically using a one‐way analysis of variance and post hoc Tukey's test at the 5% significant level. There was no significant difference between the new and used D1 and D2 PTUR and WOG instruments in terms of the Ni composition (p > .05). The Ti contents of the used D2 and D3 PTUR instruments were lower those of the new instruments (p < .05). In both new and used instruments, PTUR and WOG have no difference in terms of Ra and RMS values. (p > .05). The Ra and RMS values of the PTUR and WOG systems significantly increased after removal of the root canal filling (p < .05). The use of PTUR and WOG instruments for removal of root canal filling in severely curved root canals affected the surface topography of the files. The NiTi composition of the WOG instruments was unaffected by the retreatment process.     

Defects formed within hardness indenter interaction zone in Al2O3–ZrO2 composite

The Al₂O₃?10 wt% ZrO₂ composites were subjected to hardness tests using a Vickers diamond indenter up to 98.1 N. The microstructure observation using a transmission electron microscopy technique helped to identify up to four zones differing in defect level and character. The densest dislocation tangles, twins accumulation and frequent presence of three slip systems were found in regions that were in contact with the sides of the diamond pyramid. The second zone, characterized by two, or at least one, active slip systems, started at the bottom of the indentation mark and extended up to a distance comparable with the depth of indentation. In the third zone, with a thickness comparable to that above, only some α‐Al₂O₃ crystallites showed the presence of dislocations, whereas other crystallites were defect free. In the last zone the alumina crystals were left unaffected but the ZrO₂ crystallites showed twinning characteristic of strain‐induced transformation.     

Tribological behaviour of steel‐alumina sliding pairs under boundary lubrication conditions

The tribological behaviour of oil‐lubricated steel‐alumina sliding pairs was investigated using a ball‐on‐disc tribometer at room temperature. Commercial bearing balls of 10 mm diameter were mated to 99.7% Al₂O₃ discs, and additive‐free mineral oil was fed into the contact area. The sliding speed and the applied normal load were varied, and the initial surface roughness of the Al₂O₃ disc was altered using different polishing and grinding procedures. The results showed that the surface roughness of the ceramic discs dominated the tribological behaviour under the given experimental conditions. The sliding speed as well as the normal load showed less effect on the friction behaviour, but the amount of wear depended strongly on the normal load. From the results it was concluded that improvement of the surface roughness and optimised surface machining of the ceramic material can be essential for improving the tribological performance for boundary‐lubricated steel‐ceramic sliding pairs.     

Atomic force microscopy imaging of polycrystalline CuInSe2 thin films

In this study, atomic force microscopy (AFM) imaging has been used to study the structural properties of polycrystalline CuInSe₂ films, which are widely used as absorber materials in thin film solar cell devices. This technique demonstrated an excellent capability for the reproducible imaging of these rough polycrystalline materials. AFM imaging in combination with statistical analysis revealed distinct differences in the structural properties (i.e. grain width and height distributions, root‐mean‐square (RMS) and peak to valley (R_(p–v)) roughness values) as a function of the specific growth technique used and the bulk composition of the films. In the case of Cu‐rich films, prepared by the H₂Se/Ar treatment of Cu/In/Cu alloys, rough surface structures were in general observed. Statistical analysis revealed two distinct distribution of grains in these samples (1.0–2.5 μm and 3–5.5 μm) with large RMS and R_(p–v) roughness values of 380 nm and 2.6 μm, respectively. In‐rich films were characterized by the presence of much smaller, roughly circular clusters with a significant reduction in both the width and height distributions as well as RMS and R_(p–v) roughness values. The most successful growth techniques, in terms of producing homogeneous and dense films, were in the cases of H₂Se/Ar treated metallic InSe/Cu/InSe alloys and the coevaporation of all materials to form CuInSe₂. Both these techniques produced absorber films with very narrow grain width and height distributions as well as small roughness values. It was possible to establish that high efficiency devices are associated with the use of absorber films with narrow width distributions between 0.5 and 2 μm and small RMS (> 300 nm) roughness values. These values are used as a figure of merit in our laboratories to evaluate the structural properties of our CuInSe₂ thin films.     

Detecting changes in arthritic fibroblast‐like synoviocytes using atomic force microscopy

The morphological and quantitative differences between arthritic fibroblast‐like synoviocytes (FLS) and normal FLS were determined as an effective diagnostic tool for rheumatoid arthritis (RA), and confirmed using atomic force microscopy (AFM). Collagen‐induced arthritic (CIA) mice and normal mice were prepared and FLS were isolated by enzymatic digestion from the synovial tissue of sacrificed mice at 5‐week and 8‐week pathogenesis periods. Analysis of cell morphology using AFM revealed that the surface roughness around the nucleus and around the branched cytoplasm was significantly higher in CIA FLS (P < 0.05) than that in normal FLS. In addition, the roughness of two different sites on the arthritic FLS increased with an increase in the duration of pathogenesis. These results strongly suggest that AFM can be widely used as a diagnostic tool in cytopathology to detect the early signs of RA and various others diseases at the intercellular level. Microsc. Res. Tech. 78:982–988, 2015. © 2015 Wiley Periodicals, Inc.     

Wear properties of two-phase Al2O3/ZrO2 (Y2O3) ceramics at temperatures from 296 to 1073 K

Reciprocating sliding friction experiments were conducted with various two-phase, directionally solidified Al₂O₃/ZrO₂ (Y₂O₃) pins sliding on B₄C flats in air at temperatures of 296, 873, and 1073 K under dry sliding conditions. Results indicate that all the Al₂O₃/ZrO₂ (Y₂O₃) ceramics, from highly Al₂O₃-rich to ZrO₂-rich, exceed the main wear criterion requirement of 10⁻⁶ mm³ N⁻¹ m⁻¹ or lower for effective wear-resistant applications. Particularly, the eutectics and Al₂O₃-rich ceramics showed superior wear properties. The composition and microstructure of Al₂O₃/ZrO₂ (Y₂O₃) ceramics played a dominant role in controlling the wear and friction properties. The controlling mechanism of the ceramic wear, friction, and hardness was an intrinsic effect involving the resistance to shear fracture of heterophase bonding and cohesive bonding and the interlocking microstructures at different scales in the ceramics.     

Reciprocative sliding friction and wear properties of electrical discharge machined ZrO2‐based composites

Hot‐pressed, laboratory‐made, ZrO₂‐based composites with 40 vol. % WC, TiCN or TiN were surface finished by electrical discharge machining in order to compare their reciprocating sliding friction and wear response against WC–6wt%Co cemented carbide in unlubricated conditions. Sliding experiments were performed using a Plint TE77 pin‐on‐flat wear test rig, revealing a strong impact of the secondary phase on the tribological behaviour of the ZrO₂‐based composites. The worn surfaces and wear debris were characterised by scanning electron microscopy, energy dispersive X‐ray analysis and surface topography scanning, pointing out abrasion, polishing and adhesion as main wear mechanisms. The most favourable friction and wear characteristics were encountered with ZrO₂–WC composites compared to the other grades with equal amount of volumetric secondary phase. Copyright © 2009 John Wiley & Sons, Ltd.     

Topographic characterization of unworn contact lenses assessed by atomic force microscopy and wavelet transform

This paper analyses the three‐dimensional (3‐D) surface morphology of optic surface of unworn contact lenses (CLs) using atomic force microscopy (AFM) and wavelet transform. Refractive powers of all lens samples were 2.50 diopters. Topographic images were acquired in contact mode in air‐conditioned medium (35% RH, 23°C). Topographic measurements were taken over a 5 µm × 5 µm area with 512 pixel resolution. Resonance frequency of the tip was 65 kHz. The 3‐D surface morphology of CL unworn samples revealed (3‐D) micro‐textured surfaces that can be analyzed using (AFM) and wavelet transform. AFM and wavelet transform are accurate and sensitive tools that may assist CL manufacturers in developing CLs with optimal surface characteristics. Microsc. Res. Tech. 78:1026–1031, 2015. © 2015 Wiley Periodicals, Inc.     

A comparison of surface roughness of pipes as measured by two profilometers and atomic force microscopy

The objective of this study was to develop a reliable method for the measurement of pipe surface roughness. Roughness of coated pipe was measured with two linear surface profilers, a Dektak³ST® and a Hommel T 1000, and a Dimension 3000® atomic force microscope (AFM). Arithmetic roughness (R_a), root mean square roughness (R_q), and mean peak‐to‐valley height (R_ZD) were statistically analyzed. Each instrument yielded reliable results, but there were significant differences between the AFM and the other two instruments. The ability of R_ZD to ignore intermediate height data while focusing on extreme height data made it a useful parameter for detecting differences in height that would be the most likely to affect fluid flow in pipes.     

In situ synthesis and hydrothermal crystallization of nanoanatase TiO2–SiO2 coating on aramid fabric (HTiSiAF) for UV protection

TiO₂–SiO₂ thin film was prepared by sol‐gel method and coated on the aramid fabric to prepare functional textiles. The aramid fabric was dipped and withdrawn in TiO₂–SiO₂ gel and hydrothermal crystallization at 80^°C, then its UV protection functionality was evaluated. The crystalline phase and the surface morphology of TiO₂–SiO₂ thin film were characterized using SEM, XRD, and AFM respectively. SEM showed hydrothermal crystallization led to a homogeneous dispersion of anatase nonocrystal in TiO₂–SiO₂ film, and XRD suggested the mean particle size of the formed anatase TiO₂ was less than 30 nm. AFM indicated that hydrothermal treatment enhanced the crystallization of TiO₂. UV protection analysis suggested that the hydrothermally treated coated textile had a better screening property in comparison with TiO₂–SiO₂ gel and native aramid fabric. Microsc. Res. Tech. 78:918–925, 2015. © 2015 Wiley Periodicals, Inc.     

Comparisons of the topographic characteristics and electrical charge distributions among Babesia‐infected erythrocytes and extraerythrocytic merozoites using AFM

Tick‐borne Babesia parasites are responsible for costly diseases worldwide. Improved control and prevention tools are urgently needed, but development of such tools is limited by numerous gaps in knowledge of the parasite–host relationships. We hereby used atomic force microscopy (AFM) and frequency‐modulated Kelvin probe potential microscopy (FM‐KPFM) techniques to compare size, texture, roughness and surface potential of normal and infected Babesia bovis, B. bigemina and B. caballi erythrocytes to better understand the physical properties of these parasites. In addition, AFM and FM‐KPFM allowed a detailed view of extraerythrocytic merozoites revealing shape, topography and surface potential of paired and single parasites. B. bovis‐infected erythrocytes display distinct surface texture and overall roughness compared to noninfected erythrocytes. Interestingly, B. caballi‐infected erythrocytes do not display the surface ridges typical in B. bovis parasites. Observations of extraerythrocytic B. bovis, B. bigemina and B. caballi merozoites using AFM revealed differences in size and shape between these three parasites. Finally, similar to what was previously observed for Plasmodium‐infected erythrocytes, FM‐KPFM images reveal an unequal electric charge distribution, with higher surface potential above the erythrocyte regions that are likely associated with Babesia parasites than over its remainder regions. In addition, the surface potential of paired extraerythrocytic B. bovis Mo7 merozoites revealed an asymmetric potential distribution. These observations may be important to better understand the unique cytoadhesive properties of B. bovis‐infected erythrocytes, and to speculate on the role of differences in the distribution of surface charges in the biology of the parasites.     

Dislocations in nanostructured two‐phase Fe30Ni20Mn20Al30

In a previous study, the dislocations in Fe₃₀Ni₂₀Mn₂₅Al₂₅ (at. %), which consist of 50 nm wide alternating b.c.c. and B2 phases, were shown to have a/2<111> Burgers vectors after room temperature deformation. The dislocations were found to glide in pairs on both {110} and {112} slip planes and were relatively widely separated in the b.c.c. phase, where the dislocations were uncoupled, and closely spaced in the B2 phase, where the dislocations were connected by an anti‐phase boundary. In this article, we analyze the dislocations in the two ～5 nm‐wide B2 phases in a related two‐phase alloy Fe₃₀Ni₂₀Mn₂₀Al₃₀, with compositions Fe‐23Ni‐21Mn‐24Al and Fe‐39Ni‐12Mn‐34Al, compressed to ～3% strain at a strain rate 5 × 10^?4 s^?1 at 873 K (the lowest temperature at which substantial plastic flow was observed). It is shown that slip occursby the glide of a<100> dislocations. A review of the literature suggests that the differences in the observed slip vector between these B2 phases could be due to the differences in composition, differences in deformation temperature, or possibly both. Microsc. Res. Tech. 76:263–267, 2013. © 2013 Wiley Periodicals, Inc.     

Stress and strain distribution in demineralized enamel: A micro‐CT based finite element study

Physiological oral mechanical forces may play a role on the progression of enamel carious lesions to cavitation. Thus, the aim of this study was to describe, by 3D finite element analysis, stress, and strain patterns in sound and carious enamel after a simulated occlusal load. Micro‐CT based models were created and meshed with tetrahedral elements (based on an extracted third molar), namely: a sound (ST) and a carious tooth (CT). For the CT, enamel material properties were assigned according to the micro‐CT gray values. Below the threshold corresponding to the enamel lesion (2.5 g/cm³) lower and isotropic elastic modulus was assigned (E = 18 GPa against E₁ = 80 GPa, E₂ = E₃ = 20 GPa for sound enamel). Both models were imported into a FE solver where boundary conditions were assigned and a pressure load (500 MPa) was applied at the occlusal surface. A linear static analysis was performed, considering anisotropy in sound enamel. ST showed a more efficient transfer of maximum principal stress from enamel to the dentin layer, while for the CT, enamel layer was subjected to higher and concentrated loads. Maximum principal strain distributions were seen at the carious enamel surface, especially at the central fossa, correlating to the enamel cavity seen at the original micro‐CT model. It is possible to conclude that demineralized enamel compromises appropriate stress transfer from enamel to dentin, contributing to the odds of fracture and cavitation. Enamel fracture over a dentin lesion may happen as one of the normal pathways to caries progression and may act as a confounding factor during clinical diagnostic decisions. Microsc. Res. Tech. 78:865–872, 2015. © 2015 Wiley Periodicals, Inc.