Investigation of deposition temperature effect on spatial patterns of MgF2 thin films.

In this work, the atomic force microscopy (AFM) technique was used to characterize 3D MgF2 thin film surfaces through advanced analysis involving morphological, fractal, multifractal, succolarity, lacunarity and surface entropy (SE) parameters, consistent with ISO 25178-2: 2012. Samples were synthesized by electron beam deposition, grown in three different temperatures. Three different temperatures of 25°C (laboratory temperature), 150 and 300°C were chosen. The temperature of 300°C is usually the highest temperature that can be deposited with the electron beam evaporation coating system. The substrates were made of glass (diameter 16 mm, thickness 3 mm), and the samples were prepared at a pressure of 5 × 10-5  Torr. The statistical results from the AFM images indicate that topographic asperities decrease with increasing deposition temperature, showing a decrease in roughness values. Regardless of the deposition temperature, all surfaces have a self-similar behavior, presenting a very linear PSD distribution, and, according to our results, the sample deposited at 300° had the highest spatial complexity. On the other hand, surface percolation is increasing when temperature increases, indicating that its low roughness and high spatial complexity play an important role on the formation of their most percolating surface microtexture. Our results demonstrate that the lower deposition temperature promoted the formation of less discontinuous height distributions in the MgF2 films.

New Physico-Chemical Analysis of Magnesium-Doped Hydroxyapatite in Dextran Matrix Nanocomposites.

The new magnesium-doped hydroxyapatite in dextran matrix (10MgHApD) nanocomposites were synthesized using coprecipitation technique. A spherical morphology was observed by scanning electron microscopy (SEM). The X-ray diffraction (XRD) characterization results show hydroxyapatite hexagonal phase formation. The element map scanning during the EDS analysis revealed homogenous distribution of constituent elements of calcium, phosphor, oxygen and magnesium. The presence of dextran in the sample was revealed by Fourier transform infrared (FTIR) spectroscopy. The antimicrobial activity of the 10MgHAPD nanocomposites was assessed by in vitro assays using Staphylococcus aureus ATCC 25923, Pseudomonas aeruginosa ATCC 27853, Streptococcus mutans ATCC 25175, Porphyromonas gingivalis ATCC 33277 and Candida albicans ATCC 10231 microbial strains. The results of the antimicrobial assays highlighted that the 10MgHApD nanocomposites presented excellent antimicrobial activity against all the tested microorganisms and for all the tested time intervals. Furthermore, the biocompatibility assays determined that the 10MgHApD nanocomposites did not exhibit any toxicity towards Human gingival fibroblast (HGF-1) cells.

Biodefensive Based on Piper nigrum Essential Oil for Controlling of Anopheles aquasalis Larvae: Influence of Temperature (35 °C) and Preservatives.

Considerable efforts have been spent on the development of biodefensives based on the encapsulation of essential oils for controlling of urban pests from their larval stage, especially as anopheline controlling agents. The larval source management of Anopheles aquasalis is important for malaria prevention. For this reason, this research proposes larvicidal biodefensives based on polymeric particles loaded with Piper nigrum essential oil, considering the influence of temperature (35 °C) and preservatives on the formulation stability. The biodefensive containing the preservative phenoxyethanol/methylisothiazolinone (PNE) resulted in 5 months of shelf-life storage with an Encapsulation Efficiency (EE%) of essential oil of 70%. The biodefensive PNE (containing 500 µg.mL-1 of encapsulated essential oil) presented a polydisperse particle size distribution, ranging from D10 = (127 ± 10) nm to D90 = (472 ± 78) nm and a particle mean size of (236 ± 34) nm. The AFM images revealed a spherical morphology with an external surface almost regular and smooth. The controlled release of the essential oil was evaluated up to 72 h according to the Korsmeyer-Peppas mathematical model, confirming the anomalous transport (n = 0.64 in pH = 3 and pH = 10, and n = 0.65 in pH = 7). The total larvae mortality on the in loco bioassays was almost reached (92%) after 24 h. However, according to the in vitro bioassays applying the in natura essential oil alone, the concentration of 454 µg.mL-1 resulted on the mortality of 70% of the larvae after 24 h. For this reason, the highest efficiency of the biodefensive PNE may be related to the encapsulation of essential oil, delivering the loaded particles more efficiently inside the larvae. From this perspective, the present study shows that a formulation based on P. nigrum essential oil may be taken into account in the integrated management of disease vector mosquitoes.

Alternative Controlling Agent of Theobroma grandiflorum Pests: Nanoscale Surface and Fractal Analysis of Gelatin/PCL Loaded Particles Containing Lippia origanoides Essential Oil.

A new systematic structural study was performed using the Atomic Force Microscopy (AFM) reporting statistical parameters of polymeric particles based on gelatin and poly-ε-caprolactone (PCL) containing essential oil from Lippia origanoides. The developed biocides are efficient alternative controlling agents of Conotrachelus humeropictus and Moniliophtora perniciosa, the main pests of Theobroma grandiflorum. Our results showed that the particles morphology can be successfully controlled by advanced stereometric parameters, pointing to an appropriate concentration of encapsulated essential oil according to the particle surface characteristics. For this reason, the absolute concentration of 1000 µg·mL-1 (P1000 system) was encapsulated, resulting in the most suitable surface microtexture, allowing a faster and more efficient essential oil release. Loaded particles presented zeta potential around (-54.3 ± 2.3) mV at pH = 8, and particle size distribution ranging from 113 to 442 nm. The hydrodynamic diameter of 90% of the particle population was found to be up to (405 ± 31) nm in the P1000 system. The essential oil release was evaluated up to 80 h, with maximum release concentrations of 63% and 95% for P500 and P1000, respectively. The best fit for the release profiles was obtained using the Korsmeyer-Peppas mathematical model. Loaded particles resulted in 100% mortality of C. humeropictus up to 48 h. The antifungal tests against M. perniciosa resulted in a minimum inhibitory concentration of 250 µg·mL-1, and the P1000 system produced growth inhibition up to 7 days. The developed system has potential as alternative controlling agent, due to its physical stability, particle surface microtexture, as well as pronounced bioactivity of the encapsulated essential oil.

Effect of the Deposition Time on the Structural, 3D Vertical Growth, and Electrical Conductivity Properties of Electrodeposited Anatase-Rutile Nanostructured Thin Films.

TiO2 time-dependent electrodeposited thin films were synthesized using an electrophoretic apparatus. The XRD analysis revealed that the films could exhibit a crystalline structure composed of ~81% anatase and ~6% rutile after 10 s of deposition, with crystallite size of 15 nm. AFM 3D maps showed that the surfaces obtained between 2 and 10 s of deposition exhibit strong topographical irregularities with long-range and short-range correlations being observed in different surface regions, a trend also observed by the Minkowski functionals. The height-based ISO, as well as specific surface microtexture parameters, showed an overall decrease from 2 to 10 s of deposition, showing a subtle decrease in the vertical growth of the films. The surfaces were also mapped to have low spatial dominant frequencies, which is associated with the similar roughness profile of the films, despite the overall difference in vertical growth observed. The electrical conductivity measurements showed that despite the decrease in topographical roughness, the films acquired a thickness capable of making them increasingly insulating from 2 to 10 s of deposition. Thus, our results prove that the deposition time used during the electrophoretic experiment consistently affects the films' structure, morphology, and electrical conductivity.

Nanoscale surface dynamics of spatial patterns of polymeric bilayered particles loaded with essential oil.

Gelatin/PCL bilayered particles loaded with Piper nigrum essential oil was synthesized aiming to access their morphological and surface dynamic patterns. Atomic force microscopy (AFM) was applied to investigate the 3D morphology and multifractal aspects of the particles surface. The AFM maps revealed spherical surfaces and well dispersed particles, besides a rougher surface on the loaded system. Minkowski functionals showed that shape of the rough peaks was similar in the unloaded and loaded systems; however, the presence of deep valleys on the loaded particles revealed their rougher pattern. Multifractal analysis revealed that unloaded and loaded particles presented multifractal behavior with different surface dynamics. The loaded surface presented a greater width of the multifractal spectrum and smaller difference of fractal dimensions, confirming their more vertically growing. These results can be useful in the development of novel polymeric-based particles loaded with essential oil. Their unique surface dynamics can provide enhanced physical properties and performance in emerging biotechnological applications.

Advanced microstructure, morphology and CO gas sensor properties of Cu/Ni bilayers at nanoscale.

In this study, we investigated the morphology of synthesized Cu/Ni nanoparticles in trace of carbon sources by the co-deposition process of RF sputtering and RF-PECVD methods and localized surface plasmon resonance of CO gas sensing of Cu/Ni nanoparticles. The surface morphology was studied by analyzing 3D micrographs of atomic force microscopy using image processing techniques and fractal/multifractal analyses. The MountainsMap® Premium software with the two-way ANOVA (Variance analysis) and least-significant differences tests were used for statistical analysis. The surface nano-patterns have a local and global particular distribution. Experimental and simulated Rutherford backscattering spectra confirm the quality of nanoparticles. Then, prepared samples were exposed to CO gas flue to study their gas sensor application using the localized surface plasmon resonance method. Increasing the Ni layer over Cu one shows an interesting result in both morphology and gas sensing sides. Advanced stereometric analyses for the surface topography of thin films in conjunction with Rutherford backscattering spectrometry and Spectroscopic analysis make a unique study in the field.

Three-Dimensional Nanoscale Morphological Surface Analysis of Polymeric Particles Containing Allium sativum Essential Oil.

Biodegradable particles were developed using poly-ε-caprolactone and gelatin carriers containing different concentrations of Allium sativum essential oil (EO) (360 µg/mL, 420 µg/mL, and 460 µg/mL). Atomic force microscopy was useful to evaluate the particles' surface based on morphological parameters. The particles' size varied from 150 nm to 300 nm. The diameter was related to the increase of the particles' height as a function of the EO concentration, influencing the roughness of the surface core values (from 20 to 30 nm) and surface irregularity. The spatial parameters Str (texture aspect ratio) and Std (texture direction) revealed low spatial frequency components. The hybrid parameters Sdq (root mean square gradient) and Sdr (interfacial area ratio) also increased as a function of the EO concentration, revealing fewer flat particles. On the other hand, the functional parameters (inverse areal material ratio and peak extreme height) suggested differences in surface irregularities. Higher concentrations of EO resulted in greater microtexture asperity on the particles' surface, as well as sharper peaks. The nanoscale morphological surface analysis allowed the determination of the most appropriate concentration of encapsulated EO, influencing statistical surface parameters.

Investigation of the morphological and fractal behavior at nanoscale of patterning lines by scratching in an atomic force microscope.

In this work, the topographical effect of the scratching trajectory and the feed direction on the formation of lithographed lines on the (001) InP surface was investigated using an atomic force microscope (AFM) tip-based nanomachining approach. Nanoscratching tests were carried out using the sharp face of a diamond AFM tip in contact mode. From the topographic maps obtained by AFM, several morphological and fractal parameters were obtained and analyzed. Surface morphology presented a surface smoothing for surfaces with scratches produced in [011] and [001] directions. The height parameters confirmed this behavior because scratches in [001] direction exhibited lower roughness. Moreover, this scratch direction promoted the height distribution most symmetrical and platykurtic. The other morphological parameters revealed that this direction provided a more irregular surface (smaller Smc and Sxp ), peak distribution, denser and pointed, smaller portion of material in the core, less deep furrows, higher spatial frequency components, and high isotropy. Fractal parameters revealed that FRE90 has the highest spatial complexity, it is dominated by higher spatial frequencies, and has the lowest surface percolation. Furthermore, all samples exhibited high topographic uniformity.

Stereometric analysis of Ti1- x Alx N thin films deposited by direct current/radio frequency magnetron sputtering.

A study of image analysis of Ti1-x Alx N films deposited on corning glass substrates by a direct current (DC)/radio frequency (RF) magnetron sputtering system was performed. Atomic force microscopy (AFM) data were studied to understand how the impact of the concentration of Al content influences the 3D surface morphology as well as the surface texture parameters. The results showed that the superficial morphology was modified by the increase of Al content in the Ti1-x Alx N films, as well as the surface microtexture. It has also been observed that the Ti1-x Alx N film surface with the highest aluminum (Al) doping concentration presented a similar surface morphology to pristine titanium nitride (TiN) thin films. The Abbott-Firestone curves for all films exhibited an S-like shape suggesting topographic uniformity and Gaussian distribution of heights. An increase in surface uniformity is observed with Al concentration. The characterization of the surface morphology of Ti1-x Alx N films by the evaluation of surface statistical parameters suggests that the surface topography can be adjusted by suitable doping of aluminum and offers a deeper understanding of the applicability of these films.

Microscopy-based infrared spectroscopy as a tool to evaluate the influence of essential oil on the surface of loaded bilayered-nanoparticles.

Increasing interest in nanoparticles of technological application has been improving their fabrication processes. The encapsulation of essential oils as bioactive compounds has proved to be an excellent alternative to the use of less environment friendly compounds. However, the difficulty of identifying their constitution and interaction with carrier agents have aroused scientific interest and a problem to overcome. Bilayer-based nanoparticles were developed using gelatin and poly-ε-caprolactone (PCL) aiming the encapsulation ofPiper nigrumessential oil. based on atomic force microscopy images and dynamic light scattering analysis, the size of the unloaded and loaded nanoparticles was found around (194 ± 40) and (296 ± 54) nm, respectively. The spatial patterns revealed that the surface of nanoparticles presented different surface roughness, similar shapes and height distribution asymmetry, lower dominant spatial frequencies, and different spatial complexity. Traditional infrared spectroscopy allowed the identification of the nanoparticle outermost layer formed by the gelatin carrier, but microscopy-based infrared spectroscopy revealed a band at 1742 cm-1related to the carbonyl stretching mode of PCL, as well as a band at 1557 cm-1due to the amide II group from gelatin. The combination of microscopy and spectroscopy techniques proved to be an efficient alternative to quickly identify differences in chemical composition by evaluating different functional groups in bilayer PLC/gelatin nanoparticles of technological application.

Stereometric characterization of Dinizia excelsa Ducke wood from Amazon rainforest using atomic force microscopy.

Dinizia excelsa Ducke under three different cut conditions were carefully analyzed. The morphology and stereometry of different wood cutting surfaces (longitudinal radial, longitudinal tangential, and transversal) were studied by SEM and AFM. The results obtained in this study suggest that both the height parameters and the advanced stereometric parameters of the surfaces did not reveal a significant difference, indicating that the spatial patterns do not change according to the type of cut. In this way, the surface microtexture does not vary depending on the cut type. Similarly, the Hurst's coefficients did not show any significant difference in the spectrum of the PSD fractal region. On the other hand, Minkowski functionals presented a morphological difference between the samples. These results showed that the microtexture of the wood surface does not change as a function of the type of cut submitted to the same polishing process.

Nanoscale morphology and fractal analysis of TiO2 coatings on ITO substrate by electrodeposition.

In this paper, we introduced an advanced discussion of the 3D morphology of TiO2 coatings deposited on ITO substrate by electrodeposition under different deposition times. Atomic force microscopy was applied for obtaining topographic images of the samples. The images were processed using the MountainsMap 8.0 commercial software according to ISO 25178-2:2012. Moreover, fractal theory was applied to study the surface microtexture of coatings. The morphology was affected by the deposition time, where the grain size decreased with the increase of the time, making film's surfaces smoother. In addition, the surface roughness exhibited a random behaviour, but does not presented significant difference between samples. The fractal dimension showed similar values for all coatings. In contrast, surface texture isotropy also exhibited random behaviour. However, advanced fractal parameters revealed that when the deposition time increased, the coatings microtexture has become uniform and less porous. Furthermore, all coatings presented high topographic uniformity, regardless of deposition time. These results revealed that the morphology and microtexture of TiO2 -based coatings can be controlled by the deposition time. LAY DESCRIPTION: An advanced characterization on the micromorphology of 3D morphology, using AFM images, of Titanium dioxide (TiO2 ) coatings deposited on ITO substrate by electrodeposition under different deposition times. TiO2 is one of the most studied semiconductors to make photovoltaic devices. The versatility of this semiconductor is associated with low toxicity, high photochemical stability, abundance, and the facility to obtain by conventional synthesis routes. The obtention of a homogeneous and stable layer in the semiconductor TiO2 film deposition is a crucial stage in the assembly of sensitized photovoltaic devices. Atomic Force Microscopy (AFM) is a technique which can magnify up to a billion times and it uses a tip or probe which touches the sample surface point by point. The tip deflection is interpreted as the surface topography by the software, producing 2D or 3D images that generate several tribological parameters such as roughness in respect to a scanned area, has been a technique widely reported in the morphological characterization, determination of thickness, roughness, and particle size in thin films. Therefore, in this paper, the morphology was studied by atomic force microscopy using MountainsMap commercial software. The main goal was to study the influence of the deposition time on the morphology and microtexture of the material. New parameters such as surface entropy, fractal succolarity and fractal lacunarity were obtained for studying coatings microtexture's complexity.

Advanced Microtexture Study of Anacardium occidentale L. Leaf Surface From the Amazon by Fractal Theory.

This work applies stereometric parameters and fractal theory to characterize the structural complexity of the 3D surface roughness of Anacardium occidentale L. leaf using atomic force microscopy (AFM) measurements. Surface roughness was studied by AFM in tapping mode, in air, on square areas of 6,400 and 10,000 µm2. The stereometric analyses using MountainsMap Premium and WSXM software provided detailed information on the 3D surface topography of the samples. These data showed that the morphology of the abaxial and adaxial side of the cashew leaf is different, which was also observed in relation to their microtextures. Fractal analysis showed that the adaxial and abaxial sides have strong microtexture homogeneity, but the adaxial side presented higher surface entropy. These results show that image processing associated with fractal theory can be an indispensable tool for identifying plant species by their leaves because this species has singularities on each side of the leaf.

Stereometric characterization of kefir microbial films associated with Maytenus rigida extract.

The aim of this study was to report the first discussion of statistical parameters and possible applications related to the surface of kefir biofilms prepared with Maytenus rigida Mart. extract through micromorphology, using atomic force microscopy (AFM). Four different samples were produced. The reference contained demerara sugar with a concentration of 40 g/L and the others had added extract whose concentrations were 0.25, 0.50, and 0.75 g/L, respectively. AFM was used to image the surface in tapping mode, on square areas of 30 µm × 30 µm. Images were studied by the MountainsMap premium commercial software. The main parameter of the surface, roughness, grew with the increase of the extract concentration up to 0.50 g/L. In addition, asymmetry and kurtosis showed that the biofilm with the best peak distribution was the one with 0.25 g/L of plant extract. The other parameters followed the main results for the surface and were observed for the depth and volume parameters. The power spectrum density spectrum confirmed the reliability of the results for the sample with 0.25 g/L. Therefore, the sample with 0.25 g/L of plant extract produced the best balance in relation to the surface properties. These results showed that the biofilm morphology and microtexture were affected by the incorporation of the plant extract and can be useful to define possible applications.