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1.
J Microsc ; 290(2): 106-116, 2023 May.
Artigo em Inglês | MEDLINE | ID: mdl-36861397

RESUMO

The composition, structural features, surface morphology, roughness parameters, particle size, and magnetic features of nanostructured Fe-Co-Ni deposits manufactured on conducting indium tin oxide-coated glasses at various electrolyte pH values are studied. The deposit produced at low electrolyte pH contains slightly higher Fe and Co contents but lower Ni content compared to deposits fabricated at high pH values. Further composition analysis confirms that the reduction rates of Fe2+ and Co2+ are higher than the Ni2+ reduction rate. The films consist of nano-sized crystallites with a strong [111] preferred orientation. The results also reveal that the crystallization of the thin films is affected by the electrolyte pH. Surface analysis shows that the deposit surfaces are composed of nano-sized particles with different diameters. The mean particle diameter and surface roughness decrease as the pH of the electrolyte decreases. The effect of the electrolyte pH on the morphology is also discussed in terms of surface skewness and kurtosis parameters. Magnetic analysis shows that the resultant deposits have in-plane hysteresis loops with low and close SQR parameters ranging from 0.079 to 0.108. The results also reveal that the coercive field of the deposits increases from 29.4 Oe to 41.3 Oe as the electrolyte pH decreases from 4.7 to 3.2.

2.
J Microsc ; 287(2): 69-80, 2022 Aug.
Artigo em Inglês | MEDLINE | ID: mdl-35665928

RESUMO

The stereometric and fractal concepts are crucial tools to analyse, to verify, to report 3-D microtexture of thin film surfaces on the nanometre scale and thereby to generate useful topographic characteristics for better understanding and steering them toward further improvements and rational use in modern applications. At first, the present work aimed to prepare hematite α-Fe2 O3 thin films with (0, 2, 4, 6 and 8 wt%) of Cu doping by using the air pneumatic spray method. Subsequently, the obtained pure α-Fe2 O3 and Cu-doped α-Fe2 O3 thin films were characterised by XRD device, which determines their polycrystalline nature with the rhombohedral hematite structure. Analysis by UV-VIS absorption showed that the transmittance of the thin films is extinct in the wavelength from approximately 500 to 800 nm, revealing that the films have good optical absorbance in the visible region. The obtained bandgap values varied between 2.23 and 2.21 eV. At second stage, the stereometric and fractal analysis are applied on 3-D image data of pure α- Fe2 O3 and Cu-doped α-Fe2 O3 thin films, which in prior generated using AFM device. Accordingly, the obtained statistical parameters such as surface roughness, density distribution of peaks, depths etc. were used to understand the influence of Cu doping on the 3D microtexture of pure α- Fe2 O3 and Cu-doped α- Fe2 O3 thin film surfaces.

3.
Molecules ; 27(19)2022 Sep 20.
Artigo em Inglês | MEDLINE | ID: mdl-36234682

RESUMO

In this work, the optical properties of tetra(imidazole) of palladium phthalocyanine (PdPc(Im)4) in solution form and thin films on glass and fluorine-doped tin oxide (FTO) substrates were investigated via the thermal evaporation technique. The optical band gap was evaluated by ultraviolet-visible spectroscopy (UV-Vis). The energy band gap values were determined based on the Tauc graph. In addition, time-dependent density functional theory (TD-DFT) was used to simulate the UV-Vis absorption spectrum of the (PdPc(Im)4) molecule in the Dimethyl Sulfoxide (DMSO) solution phase. A good correlation was found between the DFT results and the experimental optical results. The band gap values between the experimental and DFT-simulated values are presented. The energy band gap of (PdPc(Im)4) obtained from the DFT calculations showed that it can be efficiently regulated. Frontier molecular orbitals and molecular electrostatic potentials were also proposed in this work. The surface study of the layers deposited on FTO was considered by atomic force microscopy (AFM) and scanning electron microscopy (SEM), and the results demonstrated good homogeneity covering the entire surface. The SEM image showed a homogeneous distribution of the grains with some spherical or rod-shaped structures and no agglomeration structures. This work rendered a strategy for regulating the energy band gap and compared the experimental observations obtained with theoretical studies, which provides a fundamental insight into the optical band for optoelectronic and thin-film solar cells.

4.
Molecules ; 27(19)2022 Sep 27.
Artigo em Inglês | MEDLINE | ID: mdl-36234901

RESUMO

Bromelain has potential as an analgesic, an anti-inflammatory, and in cancer treatments. Despite its therapeutic effects, this protein undergoes denaturation when administered orally. Microencapsulation processes have shown potential in protein protection and as controlled release systems. Thus, this paper aimed to develop encapsulating systems using sodium alginate as a carrier material and positively charged amino acids as stabilizing agents for the controlled release of bromelain in in vitro tests. The systems were produced from the experimental design of centroid simplex mixtures. Characterizations were performed by FTIR showing that bromelain was encapsulated in all systems. XRD analyses showed that the systems are semi-crystalline solids and through SEM analysis the morphology of the formed systems followed a pattern of rough microparticles. The application of statistical analysis showed that the systems presented behavior that can be evaluated by quadratic and special cubic models, with a p-value < 0.05. The interaction between amino acids and bromelain/alginate was evaluated, and free bromelain showed a reduction of 74.0% in protein content and 23.6% in enzymatic activity at the end of gastric digestion. Furthermore, a reduction of 91.6% of protein content and 65.9% of enzymatic activity was observed at the end of intestinal digestion. The Lis system showed better interaction due to the increased stability of bromelain in terms of the amount of proteins (above 63% until the end of the intestinal phase) and the enzymatic activity of 89.3%. Thus, this study proposes the development of pH-controlled release systems aiming at increasing the stability and bioavailability of bromelain in intestinal systems.


Assuntos
Alginatos , Bromelaínas , Alginatos/química , Aminoácidos , Preparações de Ação Retardada , Excipientes , Projetos de Pesquisa
5.
Molecules ; 27(20)2022 Oct 18.
Artigo em Inglês | MEDLINE | ID: mdl-36296621

RESUMO

This paper presents the results of the synthesis of samarium-doped bismuth ferrite (BFO) nanoparticles by the solution combustion method. The dependence of BFO properties on the amount of the samarium (Sm) in the composition was studied. The synthesized nanocomposites were characterized by scanning electron microscopy SEM), X-ray diffractometry (XRD), Raman, Electron Diffuse Reflectance Spectroscopy (EDRS) and Electron Magnetic Resonance (EMR). The photocatalytic (PC) measurements showed the absence of a strict correlation between the PC activity and the crystallite size and band gap. An increase in the PC activity of BFO samples with 10 and 15% doping was observed and it was concluded that in controlling the PC properties in doped BFO, the processes of interfacial polarization at the boundaries of the morphotropic phase transition are of decisive importance. It was supposed that the internal electric field formed at these boundaries contributes to the efficient separation of photogenerated charge carriers.

6.
Molecules ; 27(12)2022 Jun 08.
Artigo em Inglês | MEDLINE | ID: mdl-35744819

RESUMO

Poly(o-methoxyaniline) emeraldine-salt form (ES-POMA) was chemically synthesized using hydrochloric acid and subjected to a heat treatment (HT) process for 1 h at 100 °C (TT100) and 200 °C (TT200). The HT process promoted a progressive decrease in crystallinity. The Le Bail method revealed a decomposition from tetrameric to trimeric-folded chains after the HT process. The unheated POMA-ES presented a globular vesicular morphology with varied micrometric sizes. The heat treatment promoted a reduction in these globular structures, increasing the non-crystalline phase. The boundary length (S) and connectivity/Euler feature (χ) parameters were calculated from the SEM images, revealing that ES-POMA presented a wide distribution of heights. The TT100 and TT200 presented a narrow boundary distribution, suggesting smoother surfaces with smaller height variations. The UV-VIS analysis revealed that the transition at 343 nm (nonlocal π → π*) was more intense in the TT200 due to the electronic delocalization, which resulted from the reduced polymer chain caused by the HT process. In addition to the loss of conjugation, counter ion withdrawal reduced the ion-chain interaction, decreasing the local electron density. This result shows the influence of the chlorine counter ions on the peaks position related to the HOMO → LUMO transition, since the π → polaron transition occurs due to the creation of the energy states due to the presence of counter ions. Finally, the electrical conductivity decreased after the HT process from 1.4 × 10-4 S.cm-1 to 2.4 × 10-6 S.cm-1 as result of the polymer deprotonation/degradation. Thus, this paper proposed a systematic evaluation of the POMA molecular structure and crystallite size and shape after heat treatment.


Assuntos
Temperatura Alta , Poliaminas , Compostos de Anilina , Condutividade Elétrica , Poli A , Poliaminas/química , Polímeros/química
7.
Molecules ; 27(19)2022 Sep 26.
Artigo em Inglês | MEDLINE | ID: mdl-36234863

RESUMO

Poly(p-anisidine) (PPA) is a polyaniline derivative presenting a methoxy (-OCH3) group at the para position of the phenyl ring. Considering the important role of conjugated polymers in novel technological applications, a systematic, combined experimental and theoretical investigation was performed to obtain more insight into the crystallization process of PPA. Conventional oxidative polymerization of p-anisidine monomer was based on a central composite rotational design (CCRD). The effects of the concentration of the monomer, ammonium persulfate (APS), and HCl on the percentage of crystallinity were considered. Several experimental techniques such as X-ray Diffraction (XRD), Scanning Electron Microscopy (SEM), multifractal analysis, Nuclear Magnetic Resonance (13C NMR), Fourier-transform Infrared spectroscopy (FTIR), and complex impedance spectroscopy analysis, in addition to Density Functional Theory (DFT), were employed to perform a systematic investigation of PPA. The experimental treatments resulted in different crystal structures with a percentage of crystallinity ranging from (29.2 ± 0.6)% (PPA1HT) to (55.1 ± 0.2)% (PPA16HT-HH). A broad halo in the PPA16HT-HH pattern from 2θ = 10.0-30.0° suggested a reduced crystallinity. Needle and globular-particle morphologies were observed in both samples; the needle morphology might have been related to the crystalline contribution. A multifractal analysis showed that the PPA surface became more complex when the crystallinity was reduced. The proposed molecular structures of PPA were supported by the high-resolution 13C NMR results, allowing us to access the percentage of head-to-tail (HT) and head-to-head (HH) molecular structures. When comparing the calculated and experimental FTIR spectra, the most pronounced changes were observed in ν(C-H), ν(N-H), ν(C-O), and ν(C-N-C) due to the influence of counterions on the polymer backbone as well as the different mechanisms of polymerization. Finally, a significant difference in the electrical conductivity was observed in the range of 1.00 × 10-9 S.cm-1 and 3.90 × 10-14 S.cm-1, respectively, for PPA1HT and PPA16HT-HH.


Assuntos
Polímeros , Compostos de Anilina , Cristalização/métodos , Polímeros/química , Espectroscopia de Infravermelho com Transformada de Fourier , Difração de Raios X
8.
Molecules ; 27(15)2022 Jul 31.
Artigo em Inglês | MEDLINE | ID: mdl-35956855

RESUMO

The development of conjugated polymer-based nanocomposites by adding metallic particles into the polymerization medium allows the proposition of novel materials presenting improved electrical and optical properties. Polyaniline Emeraldine-salt form (ES-PANI) has been extensively studied due to its controllable electrical conductivity and oxidation states. On the other hand, tungsten oxide (WO3) and its di-hydrated phases, such as WO3·2H2O, have been reported as important materials in photocatalysis and sensors. Herein, the WO3·2H2O phase was directly obtained during the in-situ polymerization of aniline hydrochloride from metallic tungsten (W), allowing the formation of hybrid nanocomposites based on its full oxidation into WO3·2H2O. The developed ES-PANI-WO3·2H2O nanocomposites were successfully characterized using experimental techniques combined with Density Functional Theory (DFT). The formation of WO3·2H2O was clearly verified after two hours of synthesis (PW2 nanocomposite), allowing the confirmation of purely physical interaction between matrix and reinforcement. As a result, increased electrical conductivity was verified in the PW2 nanocomposite: the DFT calculations revealed a charge transfer from the p-orbitals of the polymeric phase to the d-orbitals of the oxide phase, resulting in higher conductivity when compared to the pure ES-PANI.

9.
Molecules ; 27(18)2022 Sep 06.
Artigo em Inglês | MEDLINE | ID: mdl-36144505

RESUMO

The temperature dependence of the electrical properties of composites formed by biphasic sodium titanate and poly(o-methoxyaniline) (Na2Ti3O7/Na2Ti6O13/POMA) with different concentrations of POMA (0%, 1%, 10%, 15%, 35% and 50%) in the ceramic matrix was determined from measurements of complex impedance. The structural details were studied by means of X-ray diffraction, confirming the formation of the Na2Ti3O7/Na2Ti6O13/POMA composites. The displacement of the (200) reflection from 2θ = 10.45° to 11.15° in the composites with 10 and 15% of POMA suggested the partial replacement of H+ for Na+ in the Na2Ti3O7 structure. The thermal properties were investigated by Thermogravimetry and Differential Thermal Analysis. The Thermogravimetry curves of the composites with POMA content of 1, 10 and 15% presented profiles similar to that of pure sodium titanate sample. The composites with 35 and 50% of POMA showed a process at temperatures around 60-70 °C, which was associated with water absorbed by the polymer. The analysis of the complex impedance spectroscopy measurements revealed that the electrical resistivity of the composites in the range from 0 to 35% increased by two orders of magnitude, with different values for each concentration. This positive temperature coefficient of resistivity was less noticeable in the composite with highest POMA mass content (50%). The rapid increase in resistivity caused an increase in the relaxation time calculated from the time domain. The electrical response of the 50% of POMA compound changes in relation to what was observed in the other compounds, which suggests that there is a saturation limit in the increase in resistivity with POMA content.


Assuntos
Polímeros , Titânio , Óxidos , Polímeros/química , Ácidos Polimetacrílicos , Temperatura , Água
10.
Molecules ; 27(18)2022 Sep 15.
Artigo em Inglês | MEDLINE | ID: mdl-36144765

RESUMO

One of the most widely used molecules used for photodynamic therapy (PDT) is 5-aminolevulinic acid (5-ALA), a precursor in the synthesis of tetrapyrroles such as chlorophyll and heme. The 5-ALA skin permeation is considerably reduced due to its hydrophilic characteristics, decreasing its local bioavailability and therapeutic effect. For this reason, five different systems containing polymeric particles of poly [D, L-lactic-co-glycolic acid (PLGA)] were developed to encapsulate 5-ALA based on single and double emulsions methodology. All systems were standardized (according to the volume of reagents and mass of pharmaceutical ingredients) and compared in terms of laboratory scaling up, particle formation and stability over time. UV-VIS spectroscopy revealed that particle absorption/adsorption of 5-ALA was dependent on the method of synthesis. Different size distribution was observed by DLS and NTA techniques, revealing that 5-ALA increased the particle size. The contact angle evaluation showed that the system hydrophobicity was dependent on the surfactant and the 5-ALA contribution. The FTIR results indicated that the type of emulsion influenced the particle formation, as well as allowing PEG functionalization and interaction with 5-ALA. According to the 1H-NMR results, the 5-ALA reduced the T1 values of polyvinyl alcohol (PVA) and PLGA in the double emulsion systems due to the decrease in molecular packing in the hydrophobic region. The results indicated that the system formed by single emulsion containing the combination PVA-PEG presented greater stability with less influence from 5-ALA. This system is a promising candidate to successfully encapsulate 5-ALA and achieve good performance and specificity for in vitro skin cancer treatment.


Assuntos
Ácido Aminolevulínico , Ácido Poliglicólico , Clorofila , Emulsões , Heme , Ácido Láctico/química , Tamanho da Partícula , Polietilenoglicóis/química , Ácido Poliglicólico/química , Copolímero de Ácido Poliláctico e Ácido Poliglicólico , Álcool de Polivinil/química , Tensoativos , Tetrapirróis
11.
J Microsc ; 281(3): 190-201, 2021 Mar.
Artigo em Inglês | MEDLINE | ID: mdl-32926411

RESUMO

Till now electron microscopy techniques have not been used to evaluate the plasma-target interactions undergone during the magnetron sputtering process. The destructive nature of this interaction severely alters the target microstructure. Utilising quantitative microscopy techniques can shed light on the complex plasma and solid-state processes involved which can ultimately lead to improved functional thin film deposition. As a representative functional material, aluminium-doped-zinc oxide (AZO) is an upcoming alternative to conventional transparent electrode wherein the process optimisation is of great importance. In this paper, we evaluate the pre- and post-sputter field emission scanning electron microscopy (FESEM) data for ceramic AZO target fabricated at three final sintering temperatures (1100°C, 1200°C and 1300°C). In all cases, grain boundaries are merged in addition to a visible reduction in the secondary phases which makes segmentation-based image analysis challenging. Through surface statistics (i.e. fractal dimension, autocorrelation length, texture aspect ratio and entropy) as a function of magnification we can quantify the electron microscopy image of the microstructure. We show that the plasma-microstructure interaction leads to an increase in autocorrelation length, texture aspect ratio and entropy for the optimum AZO ceramic sputtering target sintered at 1200°C. Furthermore, a maximum reduction in fractal dimension span (as determined by exponential regression) is also observed for 1200°C. In addition to the evaluation of plasma effects on sintering, our approach can provide a window towards understanding the underlying thin film growth mechanisms. We believe that this technique can be applied to the defect characterisation of a wide range of polycrystalline ceramic sputtering targets (e.g. ITO, CZTS, GAZO and so on) with the ultimate goal of improving the magnetron sputtering process and the resulting functional thin film. LAY DESCRIPTION: Magnetron sputtering allows scientists to make functional thin films on the order of the nanoscale. In this technique, atoms are plucked from a 'target' then placed onto a substrate forming a thin nanometric film: all thanks to magnets, a special power supply and the fourth state of matter (plasma). Understanding what is going on and how to make a 'good' thin film is important for making better light emitting diodes, solar cells and light sensors. Scientists use electron microscopy to see what is going on in the microstructure of the sputtered thin films to fine tune the sputtering recipe. Here, for the first time, we have applied electron microscopy to see the surface of the microstructure before and after magnetron sputtering. This will help us understanding the plasma-microstructure interaction allowing us to make more informed decisions when fine-tuning the sputtering process to get improved thin films. This is a case study of aluminium-doped zinc oxide (AZO) target that could potentially replace indium tin oxide (ITO), which is widely used as a transparent electrode in devices involving light and electricity. In this case, improved characteristics would be lower electrical resistivity and higher transmission of light. We show that it is possible to use a mathematical description (e.g. the fractal dimension) of the scanning electron microscopy picture to show a link between the target surface and the functional properties. Simple explanation of fractal dimensions by Sixty Symbols ○ https://www.youtube.com/watch?v=cmBljeC79Ls Experimental demonstration of magnetron sputtering by The Thought Emporium ○ https://www.youtube.com/watch?v=Cyu7etM-0Ko Introductory video on magnetron sputtering by Applied Science ○ https://www.youtube.com/watch?v=9OEz_e9C4KM Demonstration of AZO target fabrication and sputtering by Pradhyut Rajjkumar ○ https://www.youtube.com/watch?v=kTLaTJfNX3c Simple explanation of a DIY SEM by Applied Science ○ https://www.youtube.com/watch?v=VdjYVF4a6iU.

12.
Int Ophthalmol ; 40(2): 459-465, 2020 Feb.
Artigo em Inglês | MEDLINE | ID: mdl-31677086

RESUMO

PURPOSE: We aim to improve contact lens fitting by using an innovative and simple photogrammetry imaging system to find the sagittal height (SAG) of soft contact lenses. METHODS: Eleven different types of commercially available soft contact lenses were measured, and five different lenses per package of each lens type were evaluated. The lenses were inserted in a polymethyl methacrylate cell with parallel faces containing a solution of saline and fluorescein to improve the contrast against the background. For every lens, two photographs from the top view and five photographs from the side view were taken. Using homothetic transformations, we calculated the sagittal height. RESULTS: The SAG of all lenses ranged from 3450 to 3907 µm. Differences can be appreciated between SAG of different materials. Performing an ANOVA test, we confirm that the intra-packaging sagitta is reliable for every lens. Comparing the measured SAG with the calculated spherical one, we confirm that the majority of lenses, eight out of eleven, have a spherical geometry for the internal side. Finally, we are able to group the type of lenses that present similar SAG apart from the data reported on the blister. CONCLUSION: Optical coherence tomography measurement of the eye sagitta over a given chord helped finding the first lens to fit, because matching contact lens sagitta and ocular sagitta is the key for a good fitting. In our work, we found that the majority of brands use single sphere geometry for internal surface of disposable soft contact lenses.


Assuntos
Lentes de Contato Hidrofílicas , Refração Ocular/fisiologia , Tomografia de Coerência Óptica/métodos , Córnea/diagnóstico por imagem , Equipamentos Descartáveis , Humanos , Ajuste de Prótese
13.
Mol Vis ; 24: 902-912, 2018.
Artigo em Inglês | MEDLINE | ID: mdl-30713427

RESUMO

PURPOSE: This study aimed to quantify the three-dimensional micromorphology of the surface of the human lens capsule as a function of age. METHODS: Imaging experiments were conducted on whole human lenses received from eight human cadavers (donor age range: 30-88 years). Imaging was performed with an atomic force microscope (AFM) in contact mode in fluid. The porosity and surface roughness were quantified from the height images obtained. A novel approach, based on stereometric and fractal analysis of three-dimensional surfaces developed for use in conjunction with AFM data, was also used to analyze the surface microtexture as a function of age. RESULTS: The AFM images obtained depict a highly ordered fibrous structure at the surface of the lens capsule, although the overall structure visually changes with age. Porosity and roughness were quantified for each image and analyzed as a function of donor age. The interfibrillar spacing revealed an increasing trend with age, although this result was not significant (p = 0.110). The root mean square (RMS) deviation and average deviation significantly decreased with increasing age (p<0.001 for both). The fractal analysis provided quantitative values for 29 amplitude, hybrid, functional, and spatial parameters. All the hybrid parameters decreased with age, although not significantly. Of the functional parameters, the surface bearing index increased significantly with age (p = 0.017) and the summit height exhibited a decreasing trend with age (p = 0.298). Of the spatial parameters, the dominant radial wavelength trend moved toward an increase with age (p = 0.103) and the cross-hatch angle tended toward a decrease with age (p = 0.213). CONCLUSIONS: Significant changes in the three-dimensional surface microtexture of the human lens capsule were found with age, although more experiments on a larger dataset are needed to conclude this with certainty. The analyzed AFM images demonstrate a fractal nature of the surface, which is not considered in classical surface statistical parameters. The surface fractal dimension may be useful in ophthalmology for quantifying human lens architectural changes associated with different disease states to further our understanding of disease evolution.


Assuntos
Imageamento Tridimensional/métodos , Cápsula do Cristalino/ultraestrutura , Adulto , Fatores Etários , Idoso , Idoso de 80 Anos ou mais , Cadáver , Feminino , Fractais , Humanos , Imageamento Tridimensional/instrumentação , Cápsula do Cristalino/anatomia & histologia , Cápsula do Cristalino/diagnóstico por imagem , Masculino , Microscopia de Força Atômica/métodos , Pessoa de Meia-Idade
14.
Bull Math Biol ; 80(11): 2856-2870, 2018 11.
Artigo em Inglês | MEDLINE | ID: mdl-30194522

RESUMO

A lot of insect families have physical structures created by evolution for coloration. These structures are a source of ideas for new bio-inspired materials. The aim of this study was to quantitatively characterize the micromorphology of butterfly wings scales using atomic force microscopy and multifractal analysis. Two types of butterflies, Euploea mulciber ("striped blue crow") and Morpho didius ("giant blue morpho"), were studied. The three-dimensional (3D) surface texture of the butterfly wings scales was investigated focusing on two areas: where the perceived colors strongly depend on and where they do not depend on the viewing angle. The results highlight a correlation between the surface coloration and 3D surface microtexture of butterfly wings scales.


Assuntos
Escamas de Animais/ultraestrutura , Borboletas/ultraestrutura , Asas de Animais/ultraestrutura , Animais , Fractais , Imageamento Tridimensional , Conceitos Matemáticos , Microscopia de Força Atômica , Modelos Biológicos , Nanoestruturas/ultraestrutura , Pigmentação , Propriedades de Superfície
15.
J Microsc ; 264(2): 198-206, 2016 11.
Artigo em Inglês | MEDLINE | ID: mdl-27312957

RESUMO

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 Str (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 Str values, which became higher, whereas the Sq 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 Dcc was found to be material- and treatment-insensitive.


Assuntos
Resinas Compostas/química , Nanocompostos/ultraestrutura , Saliva Artificial , Microscopia de Força Atômica , Propriedades de Superfície
16.
Implant Dent ; 23(3): 295-304, 2014 Jun.
Artigo em Inglês | MEDLINE | ID: mdl-24844390

RESUMO

INTRODUCTION: The aim of this study was to assess the correlation between the fractal analysis of gingival changes and systemic nitro-oxidative stress in a short-term low-dose ibuprofen (IBU) treatment at experimental peri-implantitis (PI). MATERIALS AND METHODS: Six adult male mixed-breed dogs with PI were randomly treated for 2 weeks, 3 with IBU (5 mg/kg b.w.) and 3 with placebo. Clinical and radiological evaluation were performed. Gingival biopsies were assessed by light microscopy, transmission electron microscopy, and fractal analysis. Blood was collected to assay nitric oxide (NOx), total oxidative status (TOS), total antioxidant response (TAR), and oxidative stress index (OSI). RESULTS: Specific gingival ultrastructural alterations, bone loss, and systemic nitro-oxidative stress were evident in PI-placebo animals. IBU caused significant clinical, microscopic, fractal dimensions (P < 0.01), NOx, TOS, and OSI improvements. IBU caused no important bone and TAR changes. CONCLUSION: This study confirms that fractal analysis was a good method to assess the complex morphological changes and correlations with the nitro-oxidative stress in PI. Short-term low-dose IBU treatment consistently improved gingival status and reduced systemic nitro-oxidative stress.


Assuntos
Anti-Inflamatórios não Esteroides/uso terapêutico , Ibuprofeno/uso terapêutico , Peri-Implantite/tratamento farmacológico , Animais , Cães , Fractais , Gengiva/efeitos dos fármacos , Gengiva/patologia , Gengiva/ultraestrutura , Masculino , Microscopia , Microscopia Eletrônica de Transmissão , Óxido Nítrico/sangue , Estresse Oxidativo/efeitos dos fármacos , Peri-Implantite/patologia
17.
Microsc Res Tech ; 87(8): 1974-1983, 2024 Aug.
Artigo em Inglês | MEDLINE | ID: mdl-38590286

RESUMO

As the first boundary between the environment and the material, the surface plays an important role in their interaction with each other, therefore, the use of appropriate tools and analysis to examine the mechanical properties and morphology of surfaces has particular importance in industry and research. In this research, a thin film of nickel was deposited on metal substrates made of aluminum, copper, and steel by using the RF magnetic cathode. Then, using a non-contact atomic force microscope, the morphological properties of the nickel film with static parameters, Minkowski functionals (MF's), fractal, and multifractal were extracted to be analyzed and studied. After that, using parameters such as root mean square (RMS) roughness, skewness, and kurtosis, it was determined how the surface roughness, distribution, and probability density of particles on the film surface alters with the change of the substrate. Next, by examining and analyzing the Δα and Δf parameters obtained from the multifractal section, the morphology of the produced film on the metal substrates was investigated. Then, the change in the surface plasmon resonance (SPR) peak position is changed for the prepared film in the range of the absorption spectrum due to the substrate effect and the microstructural properties of the formed film. HIGHLIGHTS: Ni film has been deposited by Rf magnetron sputtering. The effect of metal substrates on the topography, fractality, and optical properties was studied. Minkowski functionals were used to investigate the surface morphology of the samples. Substrate's material and the topography of the formed film can changed the surface plasmon resonance position.

18.
Microsc Res Tech ; 87(5): 876-887, 2024 May.
Artigo em Inglês | MEDLINE | ID: mdl-38126943

RESUMO

The principal aim of this study is to reduce considerably, via Sn doping, the resistivity of ZnO thin films prepared by simple, flexible, and cost-effective nitrogen pneumatic spray pyrolysis (NPSP) method on glass substrates at a temperature of 400°C. Different Sn content was tested (Sn/Zn = 0, 1, 3, 5 wt%) in an attempt to reduce the concentration of excessive oxygen atoms and create more free electrons. The microstructural, optical, morphological, and electrical properties of the films have been studied. The x-ray diffraction analysis demonstrated that tin-doped SZO films exhibited polycrystalline nature with a preferential orientation along (002) plane with the appearance of a new orientation (101) with the increase of Sn concentration leading then to bidirectional growth. The deposited SZO films showed an average optical transmittance of about 80% in the UV-visible region (200-800 nm) with optical band gap values at around 3.27 eV. Photoluminescence emissions of SZO samples presented three main peaks: near band edge emission, violet emission, and the blue-green emission. The surface morphology of the films obtained by scanning electron microscope (SEM) exhibited the change in morphology with increasing the Sn content. A minimum electrical resistivity value of about 17·10-3 Ω·cm was obtained for 3% SZO films. SZO films prepared by the NPSP method can be used as transparent window layer and electrodes in solar cells. RESEARCH HIGHLIGHTS: Highly oriented, conducting, and transparent Sn-doped ZnO films are successfully synthesized. The film growth orientation changed from mono-directional (002) axis to bi-directional (002) and (101) axis according to Sn doping. Ultraviolet and green emissions are noted by photoluminescence investigation. A minimum resistivity is observed for 3 wt% SZO film. The dual positive effect of the carrier gas used (N2) and Sn doping is confirmed.

19.
Microsc Res Tech ; 87(7): 1402-1412, 2024 Jul.
Artigo em Inglês | MEDLINE | ID: mdl-38380821

RESUMO

Utilizing radio frequency magnetron sputtering, we successfully fabricated nickel oxide thin films with different thickness (from 80 to 270 nm), and conducted an in-depth examination of their structural, morphological, optical, and electrical properties. The crystal structure and surface roughness were determined using x-ray diffraction (XRD) and atomic force microscopy (AFM), respectively. The XRD analyses showed that the films were composed of cubic nickel oxide, exhibiting a notable orientation along the (200) direction. This crystal texture partially increased when the film thickness reached 270 nm. In addition, a direct correlation between film thickness and crystallite size was observed, with the latter increasing as the former did. AFM analysis provided insights into the surface morphology, revealing metrics like the bearing area, 3D surfaces intersections, and statistical properties of surface height. These insights underscore the relationship between film thickness and surface properties, which in turn influence the overall electrical, and prominently, optical properties of the films. Employing transmittance UV-visible spectroscopy, we characterized the optical behavior of these films, noting a proportional increase in refractive index with film thickness. Additionally, resistivity was observed to increase concomitantly with film thickness. In conclusion, the deposition process's film thickness acts as a pivotal parameter for fine-tuning the structural, morphological, and optical properties of nickel oxide thin films. This knowledge paves the way for optimizing nickel oxide-based devices across various applications. RESEARCH HIGHLIGHTS: We synthesized and characterized of p-type semiconducting NiO thin films sputtered on substrates by using RF magnetron sputtering with different thickness. Advanced crystalline structures and fractal features extracted from XRD and AFM analysis.  The 2D and 3D surface analysis of the samples indicates a complex structure with an imperfect self-similarity that suggests a multifractal structure. We represented graphically the relative representation of higher geometric objects in the AFM image. We attributed the optical and electrical properties of the samples to the crystallite size, and the concurrent reduction in oxygen vacancies and crystalline defects within the films.

20.
Microscopy (Oxf) ; 73(1): 55-65, 2024 Feb 07.
Artigo em Inglês | MEDLINE | ID: mdl-37540558

RESUMO

We conducted a comprehensive analysis of the surface microtexture of kefir biofilms grown on Theobroma grandiflorum Shum (cupuaçu) juice using atomic force microscopy. Our goal was to investigate the unique monofractal and multifractal spatial patterns of these biofilms to complement the existing limited literature. The biofilms were prepared dispersing four different concentrations of kefir grains in cupuaçu juice. Our morphological analysis showed that the surface of the obtained biofilms is essentially formed by the presence of cupuaçu fibers and microorganisms like lactobacilli and yeast. The topographic height-based parameter analysis reveals that there is a dependence between surface roughness and the concentration of kefir grains used. The strongly anisotropic well-centralized topographical height distribution of the biofilms also exhibited a quasi-symmetrical and platykurtic pattern. The biofilms exhibit comparable levels of spatial complexity, surface percolation and surface homogeneity, which can be attributed to their similar topographic uniformity. This aspect was further supported by the presence of similar multifractality in the biofilms, suggesting that despite their varying topographic roughness, their vertical growth dynamics follow a similar pattern. Our findings demonstrate that the surface roughness of kefir biofilms cultivated on cupuaçu juice is influenced by the concentration of kefir grains in the precursor solution. However, this dependence follows a consistent pattern across different concentrations. Graphical Abstract.


Assuntos
Kefir , Biofilmes , Lactobacillus , Saccharomyces cerevisiae
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