Atomic force microscopy of anodized zirconium substrates

Atomic force microscopy (AFM) has been used to investigate the phase transitions and surface morphology transformation of cadmium mercury thiocyanate (CMTC) crystals, which are highly efficient nonlinear optical (NLO) materials for generating blue-violet light by laser frequency doubling. Amorphous aggregates at the crystalline steps become greatly contracted and much more crystalloid after the crystal was kept for one day. Elimination of dangling bonds, which lower the surface free energy at the crystal surface, and structural adjustment inside the crystal are assumed to cause this phase transition. Surface morphology transformations were also observed in CMTC crystals during and after multiple scanning by AFM tips. We have visualized the continuous translation process from two-dimensional nuclei to trigonal microcrystals with almost equal sizes during multiple scanning. In other cases, however, the surface morphology did not change at all during scanning, but became greatly altered hours after scanning. These experimental results suggest that reconstruction is a characteristic growth phenomenon on CMTC crystal surfaces. Reconstruction probably results from the formation of intervening metastable phases that have the potential to arrive at more stable stages; however, multiple scanning of AFM tips greatly affects this translation process.

Surface morphology is a key factor that determines the quality of laser-based micromachining processes. However, the governing laws of surface morphology in the laser processing process are yet to be clarified, and optimization of processing parameters has to rely on trial and error. Specifically, under multiple-pulse irradiation, it has been difficult to quantify the evolution of the surface morphology because the surface morphology changes with each pulse irradiation, and the ablation process changes accordingly. In this study, we investigated the evolution of surface morphology under femtosecond laser irradiation. Copper and silicon were used as targets, whose surface morphology changes exhibited seemingly opposite behaviors with respect to fluence. Using thousands of datasets, we obtained an evolution equation for surface morphology in terms of surface area, which acts as a good probe of the residual surface energy after ablation. Our model successfully quantifies the cumulative effect of multiple-pulse irradiation on surface morphology changes.

BackgroundCellulose amorphogenesis, described as the non-hydrolytic “opening up” or disruption of a cellulosic substrate, is becoming increasingly recognized as one of the key steps in the enzymatic deconstruction of cellulosic biomass when used as a feedstock for fuels and chemicals production. Although this process is thought to play a major role in facilitating hydrolysis, the lack of quantitative techniques capable of accurately describing the molecular-level changes occurring in the substrate during amorphogenesis has hindered our understanding of this process.ResultsIn this work, techniques for measuring changes in cellulose accessibility are reviewed and a new quantitative assay method is described. Carbohydrate binding modules (CBMs) with specific affinities for crystalline (CBM2a) or amorphous (CBM44) cellulose were used to track specific changes in the surface morphology of cotton fibres during amorphogenesis. The extents of phosphoric acid-induced and Swollenin-induced changes to cellulose accessibility were successfully quantified using this technique.ConclusionsThe adsorption of substructure-specific CBMs can be used to accurately quantify the extent of changes to cellulose accessibility induced by non-hydrolytic disruptive proteins. The technique provided a quick, accurate and quantitative measure of the accessibility of cellulosic substrates. Expanding the range of CBMs used for adsorption studies to include those specific for such compounds as xylan or mannan should also allow for the accurate quantitative tracking of the accessibility of these and other polymers within the lignocellulosic biomass matrix.

The purpose of this study was to evaluate, using scanning electron microscopy (SEM), the morphological and structural changes of the enamel induced by three bleaching agents namely old McInnes solution, modified McInnes solution and 10% carbamide peroxide gel at different time intervals. Fifteen freshly extracted noncarious human central incisors with intact enamel surface were selected. The teeth were sectioned at the cementoenamel junction separating the crown portion from the root using a diamond separating disk. Following this, the samples were subjected to three different bleaching agents: Group 1: Old McInnes solution, group 2: modified McInnes solution and group 3: 10% carbamide peroxide for a period of 15, 30 and 60 minutes, 24 and 30 hours time interval. The sample stubs were subjected to scanning electron microscope and were photographed at 2000 and 10,000 magnifications. The present study revealed no indication of either etching or significant change in surface morphology of enamel when evaluated under scanning electron microscope after 6 weeks treatment with various bleaching agents. Morphological alterations in bleached enamel are both concentration and time dependent.

Silicon carbide (SiC) and its composites are candidate materials for the blanket components and for the first wall in a fusion reactor. If the SiC is used without any armor materials for the first wall, it is exposed by helium (He) plasma as well as hydrogen plasma. Characteristic surface morphology changes are reported for various materials by He plasma exposure. Thus, we exposed SiC specimens to He or simultaneous deuterium (D) and He (D + He) plasma by various conditions and then observed surface morphology changes by SEM. As a result, needle-like structures and whiskers-like structures at the tip were formed in He plasma and D + He irradiation, while only needle-like structures were formed in D plasma. Therefore, it indicated that the effects of He were attributed to form whiskers-like structures. Although the structures are different among He plasma, simultaneous D + He plasma and D plasma irradiations, sputtering is considered to be a dominant process for the formation of the structure formation. However, the effects of He atoms in the structure could also be attributed to form whiskers-like structures.

Ultraviolet (UV) and infrared (IR) lasers can be used to specifically target protein, water, and mineral, respectively, in dental hard tissues to produce varying changes in surface morphology, permeability, reflectivity, and acid resistance. The purpose of this study was to explore the influence of laser irradiation and topical fluoride application on the surface morphology, permeability, reflectivity, and acid resistance of enamel and dentin to shed light on the mechanism of interaction and develop more effective treatments. Twelve bovine enamel surfaces and twelve bovine dentin surfaces were irradiated with various combinations of lasers operating at 0.355 (Freq.-tripled Nd:YAG (UV) laser), 2.94 (Er:YAG laser), and 9.4 μm (CO2 laser), and surfaces were exposed to an acidulated phosphate fluoride gel and an acid challenge. Changes in the surface morphology, acid resistance, and permeability were measured using digital microscopy, polarized light microscopy, near-IR reflectance, fluorescence, polarization sensitive-optical coherence tomography (PS-OCT), and surface dehydration rate measurements. Different laser treatments dramatically influenced the surface morphology and permeability of both enamel and dentin. CO2 laser irradiation melted tooth surfaces. Er:YAG and UV lasers, while not melting tooth surfaces, showed markedly different surface roughness. Er:YAG irradiation led to significantly rougher enamel and dentin surfaces and led to higher permeability. There were significant differences in acid resistance among the various treatment groups. Surface dehydration measurements showed significant changes in permeability after laser treatments, application of fluoride and after exposure to demineralization. CO2 laser irradiation was most effective in inhibiting demineralization on enamel while topical fluoride was most effective for dentin surfaces. Lasers Surg. Med. 49:913-927, 2017. © 2017 Wiley Periodicals, Inc.

Age-related changes in the surface morphology of the central sulcus

Surface morphological changes induced in catalysts by acoustic waves

HKUST-1 or Cu3BTC2 (BTC = 1,3,5-benzenetricarboxylate) is a prototypical metal-organic framework (MOF) that holds a privileged position among MOFs for device applications, as it can be deposited as thin films on various substrates and surfaces. Recently, new potential applications in electronics have emerged for this material when HKUST-1 was demonstrated to become electrically conductive upon infiltration with 7,7,8,8-tetracyanoquinodimethane (TCNQ). However, the factors that control the morphology and reactivity of the thin films are unknown. Here, we present a study of the thin-film growth process on indium tin oxide and amorphous Si prior to infiltration. From the unusual bimodal, non-log-normal distribution of crystal domain sizes, we conclude that the nucleation of new layers of Cu3BTC2 is greatly enhanced by surface defects and thus difficult to control. We then show that these films can react with methanolic TCNQ solutions to form dense films of the coordination polymer Cu(TCNQ). This chemical conversion is accompanied by dramatic changes in surface morphology, from a surface dominated by truncated octahedra to randomly oriented thin platelets. The change in morphology suggests that the chemical reaction occurs in the liquid phase and is independent of the starting surface morphology. The chemical transformation is accompanied by 10 orders of magnitude change in electrical conductivity, from <10-11 S/cm for the parent Cu3BTC2 material to 10-1 S/cm for the resulting Cu(TCNQ) film. The conversion of Cu3BTC2 films, which can be grown and patterned on a variety of (nonplanar) substrates, to Cu(TCNQ) opens the door for the facile fabrication of more complex electronic devices.

The inter–relationships of alloy composition, film composition and ionic transport for formation of amorphous anodic oxide films are addressed quantitatively through systematic study of sputter–deposited Al–Ta alloys containing up to 39 at.% Ta. The work reveals the dependence of electric field, ionic transport number, incorporation of species into the anodic film at the alloy–film interface and mobility and distribution of species within the anodic film on alloy composition. Anodic oxidation, at high current efficiency, of alloys containing 2.8, 15, 32 and 39 at.% tantalum results in formation of two–layered anodic films by migration of cations outwards and by migration of anions inwards: an outer layer, 20% or less of the total film thickness, composed of relatively pure alumina and an inner layer containing units of Al2O3 and Ta2O5 distributed relatively homogeneously. Two–layered films develop due to the slower migration rate of Ta5+ ions relative to A13+ ions in the inner layer of the growing anodic films, which changes progressively from about 0.6 for dilute alloys to about 0.9 for Al–39 at. per cent Ta. The average nm V−1 ratios, total transport numbers of cations and average Pilling–Bedworth ratios for the films change almost linearly with alloy composition between the values for anodic alumina and anodic tantala. A tantalum–enriched layer, about 1 nm thick, is formed in the Al–2.8 at.% Ta and Al–15 at.% Ta alloys just beneath the anodic film, indicating prior oxidation of aluminium in the initial stages of anodizing. In contrast, aluminium and tantalum in the alloys containing more than 30 at.% tantalum are immediately incorporated into anodic films in their alloy proportions, without development of a tantalum–enriched layer, at the available resolution. Boron species, incorporated from the electrolyte into the outer parts of the films, are immobile in films on alloys up to 15 at.% Ta but migrate outwards in other films, possibly due to the increased Lorentz field. Though the inter–relationships between film parameters and alloy composition are established for Al–Ta alloys specifically, the findings are considered to be equally relevant to amorphous anodic oxides formed on alloys and semiconductors generally.

In this work, we assess the surface modifications induced on W samples following exposure to He and He/H2 radiofrequency plasmas in hollow cathode discharge configuration. Our study addresses issues that relate to the use of W in next-generation fusion reactors and, therefore, the investigation of W surface degradation following exposure and heating by plasmas to temperatures above 1000 °C is of practical importance. For these experiments, we used commercially available tungsten samples having areas of 30 × 15 mm and 0.1 mm thickness. The hollow cathode plasma was produced using a radiofrequency (RF) generator (13.56 MHz) between parallel plate electrodes. The W samples were mounted as one of the electrodes. The He and He/H2 plasma discharges had a combined effect of heating and bombardment of the W surfaces. The surface modifications were studied for discharge powers between 200 and 300 W, which resulted in the heating of the samples to temperatures between 950 and 1230 °C, respectively. The samples were weighed prior and after plasma exposure, and loss of mass was measured following plasma exposure times up to 90 min. The analysis of changes in surface morphology was carried out by optical microscopy, scanning electron microscopy and atomic force microscopy. Additionally, optical emission spectra of the respective plasmas were recorded from the region localized inside the hollow cathode gap. We discuss the influence of experimental parameters on the changes in surface morphology.

In‐situ atomic force microscopy studies of electromigration in 4 μm wide by 1 μm thick electroplated Au wires were performed. The topographical features that develop on a sub‐micrometer length scale were studied for current densities up to 7.5×106 A/cm2 and temperatures up to 280 °C for time intervals ranging from a few minutes up to a few days. Scanning probe images of the same area taken before, during, and after current stressing reveal substantial changes in surface morphology. Both hillock growth and void formation have been observed in situ. Time lapse AFM images can be pieced together to give a microscopic picture of mass flow due to electromigration. These studies show that changes in surface morphology caused by electromigration can now be quantitatively characterized with high resolution from the scanning probe images.

The present study is aimed at investigating the change in surface morphology, hydraulic behaviour and sorption capability of two locally available Indian bentonites in the presence of different lead (Pb2+) concentrations. FESEM, FTIR, and EDX studies were conducted to analyse the change in surface morphology, alteration in FTIR pattern and decrease in exchangeable cation in both the bentonites before and after sorption of Pb2+. The tests were conducted in a batch mode to optimise operation parameters; pH, initial concentration, adsorbent dosage, and contact time. Equilibrium isotherm and sorption kinetics of both the bentonites were studied using various isotherm as well as kinetic models. The equilibrium data for both the bentonites were found to be the best fit for the Freundlich model. Both the bentonites followed Pseudo-second order equation. Hydraulic conductivity analysis illustrates that with the rise in Pb2+ concentration, the hydraulic conductivity increased for both the bentonite. The experimental evidence revealed that bentonite having high cation exchange capacity (CEC), swelling behaviour and high specific surface area (SSA) exhibits higher adsorption and heavy metal removal at 2000 mg/L of initial concentration of Pb2+ solution.

Surface appearance and morphology changes of Asian lacquer due to artificial aging: Impacts of traditional additives

Deciphering the role of second phase precipitates on early-stage surface morphology development of dispersion-strengthened W alloys under low energy He irradiation