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1.
Micron ; 184: 103661, 2024 09.
Article in English | MEDLINE | ID: mdl-38833994

ABSTRACT

The silver/magnesium doped hydroxyapatite (AgMgHAp, Ca10-x-yAgxMgy(PO4)6(OH)2, xAg=0.05 and yMg=0.02) nanocomposites coatings were deposited on Si substrate using the dip coating technique. The resulting coatings were characterized by scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), Fourier transform infrared (FTIR-ATR) spectroscopy, atomic force microscopy (AFM) and X-ray photoelectron spectroscopy (XPS). The EDS analysis highlighted the presence of the constitutive elements of the silver/magnesium doped hydroxyapatite (AgMgHAp) nanocomposites coatings. The surface microtexture of the AgMgHAp was assessed by atomic force microscopy (AFM) technique. The AFM data suggested the obtaining of a uniform deposited layer comprised of equally distributed nanoconglomerates. FT-IR studies highlighted the presence of vibrational modes associated with the phosphate and hydroxyl groups. No bands associated with silver or magnesium were observed. The XPS analysis highlighted the presence of the constituent elements of hydroxyapatite (Ca 2p, P 2 s, O 1 s), as well as dopants (Ag 3d, Mg 1 s and Mg 2p). The antifungal evaluation of AgMgHAp coatings was carried out using the Candida albicans ATCC 10231 fungal strain. The results of the antifungal assay revealed that the AgMgHAp coatings exhibited a strong inhibitory antifungal activity. Furthermore, the data highlighted that the AgMgHAp inhibited the development of biofilm on their surface. The results revealed that the antifungal activity of the coating varied based on the duration of incubation. On the other hand, the data also showed that AgMgHAp nanocomposites coatings inhibited the fungal cell adhesion and development from the early stages of the incubation. In addition to morphological analysis, we additionally take advantage of AFM images to investigate and explore the domain of fractal and multifractal analysis applied to the films under evaluation. Our studies indicates that nanocomposite coatings made from AgMgHAp demonstrate strong antifungal properties. Our studies indicates that nanocomposite coatings made from AgMgHAp demonstrate strong antifungal properties. These results suggest the potential of AgMgHAp nanocomposite coatings as a promising solution for developing innovative antifungal devices in biomedical applications.


Subject(s)
Antifungal Agents , Durapatite , Magnesium , Microscopy, Atomic Force , Nanocomposites , Silver , Durapatite/chemistry , Durapatite/pharmacology , Antifungal Agents/pharmacology , Silver/pharmacology , Silver/chemistry , Nanocomposites/chemistry , Magnesium/chemistry , Magnesium/pharmacology , Spectroscopy, Fourier Transform Infrared , Candida albicans/drug effects , Microscopy, Electron, Scanning , Photoelectron Spectroscopy , Microbial Sensitivity Tests , Spectrometry, X-Ray Emission , Coated Materials, Biocompatible/chemistry , Coated Materials, Biocompatible/pharmacology , Surface Properties
2.
Sci Rep ; 14(1): 3677, 2024 Feb 14.
Article in English | MEDLINE | ID: mdl-38355956

ABSTRACT

We investigated the multifaceted gas sensing properties of porous silicon thin films electrodeposited onto (100) oriented P-type silicon wafers substrates. Our investigation delves into morphological, optical properties, and sensing capabilities, aiming to optimize their use as efficient gas sensors. Morphological analysis revealed the development of unique surfaces with distinct characteristics compared to untreated sample, yielding substantially rougher yet flat surfaces, corroborated by Minkowski Functionals analysis. Fractal mathematics exploration emphasized that despite increased roughness, HF/ethanol-treated surfaces exhibit flatter attributes compared to untreated Si sample. Optical approaches established a correlation between increased porosity and elevated localized states and defects, influencing the Urbach energy value. This contributed to a reduction in steepness values, attributed to heightened dislocations and structural disturbances, while the transconductance parameter decreases. Simultaneously, porosity enhances the strength of electron‒phonon interaction. The porous silicon thin films were further tested as effective gas sensors for CO2 and O2 vapors at room temperature, displaying notable changes in electrical resistance with varying concentrations. These findings bring a comprehensive exploration of some important characteristics of porous silicon surfaces and established their potential for advanced industrial applications.

3.
Materials (Basel) ; 17(4)2024 Feb 08.
Article in English | MEDLINE | ID: mdl-38399069

ABSTRACT

Blast furnace dust waste (BFDW) proved efficient as a photocatalyst for the decolorization of methylene blue (MB) dye in water. Structural analysis unequivocally identified α-Fe2O3 as the predominant phase, constituting approximately 92%, with a porous surface showcasing unique 10-30 nm agglomerated nanoparticles. Chemical and thermal analyses indicated surface-bound water and carbonate molecules, with the main phase's thermal stability up to 900 °C. Electrical conductivity analysis revealed charge transfer resistance values of 616.4 Ω and electrode resistance of 47.8 Ω. The Mott-Schottky analysis identified α-Fe2O3 as an n-type semiconductor with a flat band potential of 0.181 V vs. Ag/AgCl and a donor density of 1.45 × 1015 cm-3. The 2.2 eV optical bandgap and luminescence stem from α-Fe2O3 and weak ferromagnetism arises from structural defects and surface effects. With a 74% photocatalytic efficiency, stable through three photodegradation cycles, BFDW outperforms comparable waste materials in MB degradation mediated by visible light. The elemental trapping experiment exposed hydroxyl radicals (OH•) and superoxide anions (O2-•) as the primary species in the photodegradation process. Consequently, iron oxide-based BFDW emerges as an environmentally friendly alternative for wastewater treatment, underscoring the pivotal role of its unique physical properties in the photocatalytic process.

4.
Microscopy (Oxf) ; 73(1): 55-65, 2024 Feb 07.
Article in English | MEDLINE | ID: mdl-37540558

ABSTRACT

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.


Subject(s)
Kefir , Biofilms , Lactobacillus , Saccharomyces cerevisiae
5.
Sci Rep ; 13(1): 6518, 2023 Apr 21.
Article in English | MEDLINE | ID: mdl-37085689

ABSTRACT

Due to the large number of industrial applications of transparent conductive oxides (TCOs), this study focuses on one of the most important metal oxides. The RF-magnetron sputtering method was used to fabricate NiO thin films on both quartz and silicon substrates at room temperature under flow of Argon and Oxygen. The sputtered samples were annealed in N2 atmosphere at 400, 500, and 600 °C for 2 hours. Using the AFM micrographs and WSXM 4.0 software, the basic surface parameters, including root mean square roughness, average roughness, kurtosis, skewness, etc., were computed. Advanced surface parameters were obtained by the Shannon entropy through a developed algorithm, and the power spectral density and fractal succolarity were extracted by related methods. Optical properties were studied using a transmittance spectrum to achieve the optical bandgap, absorption coefficient, Urbach energy, and other optical parameters. Photoluminescence properties also showed interesting results in accordance with optical properties. Finally, electrical characterizations and I-V measurements of the NiO/Si heterojunction device demonstrated that it can be used as a good diode device.

6.
Microsc Res Tech ; 86(2): 169-180, 2023 Feb.
Article in English | MEDLINE | ID: mdl-36260856

ABSTRACT

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.

7.
Microsc Res Tech ; 86(2): 157-168, 2023 Feb.
Article in English | MEDLINE | ID: mdl-36223516

ABSTRACT

In this study, the morphological properties and micro-roughness of chromium thin film prepared by thermal evaporation technique and confirmed via EDS analysis are examined on different substrates of BK7, Silicon (Si), and glass using atomic force microscope analysis (AFM). Analysis of amplitude parameters, Minkowski functionals, and films' spatial microtexture extracted from AFM analysis showed the difference between glass substrate and the other two (BK7 and Si) substrates for the growth of chromium thin films. In addition, we observed robust signatures of multifractality of the Cr thin films deposited on all substrates we studied. Moreover, we highlight that the Glass substrates displayed the strongest multifractality indicating that such samples present space filling properties distributed over more spatial scales than the samples of BK7 and Si.

8.
Polymers (Basel) ; 16(1)2023 Dec 29.
Article in English | MEDLINE | ID: mdl-38201790

ABSTRACT

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.

9.
Biosensors (Basel) ; 12(12)2022 Dec 13.
Article in English | MEDLINE | ID: mdl-36551128

ABSTRACT

The COVID-19 pandemic has emphasized the importance and urgent need for rapid and accurate diagnostic tests for detecting and screening this infection. Our proposal was to develop a biosensor based on an ELISA immunoassay for monitoring antibodies against SARS-CoV-2 in human serum samples. The nucleocapsid protein (N protein) from SARS-CoV-2 was employed as a specific receptor for the detection of SARS-CoV-2 nucleocapsid immunoglobulin G. N protein was immobilized on the surface of a screen-printed carbon electrode (SPCE) modified with carboxylated graphene (CG). The percentage of IgG-SARS-CoV-2 nucleocapsid present was quantified using a secondary antibody labeled with horseradish peroxidase (HRP) (anti-IgG-HRP) catalyzed using 3,3',5,5'-tetramethylbenzidine (TMB) mediator by chronoamperometry. A linear response was obtained in the range of 1:1000-1:200 v/v in phosphate buffer solution (PBS), and the detection limit calculated was 1:4947 v/v. The chronoamperometric method showed electrical signals directly proportional to antibody concentrations due to antigen-antibody (Ag-Ab) specific and stable binding reaction.


Subject(s)
Biosensing Techniques , COVID-19 , Graphite , Humans , SARS-CoV-2 , Carbon , COVID-19/diagnosis , Biosensing Techniques/methods , Pandemics , Immunoassay/methods , Nucleocapsid , Electrodes , Antibodies, Viral
10.
Biomolecules ; 12(11)2022 11 18.
Article in English | MEDLINE | ID: mdl-36421726

ABSTRACT

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.


Subject(s)
Anopheles , Oils, Volatile , Piper nigrum , Animals , Larva , Oils, Volatile/pharmacology , Temperature , Mosquito Vectors
11.
Molecules ; 27(19)2022 Sep 26.
Article in English | MEDLINE | ID: mdl-36234863

ABSTRACT

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.


Subject(s)
Polymers , Aniline Compounds , Crystallization/methods , Polymers/chemistry , Spectroscopy, Fourier Transform Infrared , X-Ray Diffraction
12.
Molecules ; 27(19)2022 Sep 27.
Article in English | MEDLINE | ID: mdl-36234901

ABSTRACT

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.


Subject(s)
Alginates , Bromelains , Alginates/chemistry , Amino Acids , Delayed-Action Preparations , Excipients , Research Design
13.
Materials (Basel) ; 15(20)2022 Oct 18.
Article in English | MEDLINE | ID: mdl-36295339

ABSTRACT

Molecularly imprinted membrane of ß-caryophyllene (MIM-ßCP) was fabricated incorporating ß-caryophyllene molecularly imprinted polymer nanoparticles (ßCP-NP) into polycaprolactone (PCL) fibers via electrospinning. The ßCP-NP were synthesized by precipitation polymerization using the ßCP as a template molecule and acrylic acid as a functional monomer in the proportion of 1:4 mol, respectively. Atomic force microscopy images and X-ray diffraction confirmed the nanoparticles' incorporation into MIM-ßCP. MIM-ßCP functionalization was evaluated by gas chromatography. The binding capacity was 1.80 ± 0.05 µmol/cm2, and the selectivity test was performed with a mixing solution of ßCP and caryophyllene oxide, as an analog compound, that extracted 77% of the ßCP in 5 min. The electrospun MIM-ßCP can be used to detect and extract the ßCP, applications in the molecular sieve, and biosensor production and may also contribute as an initial methodology to enhance versatile applications in the future, such as in the treatment of skin diseases, filters for extraction, and detection of ßCP to prevent counterfeiting of commercial products, and smart clothing with insect-repellent properties.

14.
Molecules ; 27(15)2022 Jul 31.
Article in English | MEDLINE | ID: mdl-35956855

ABSTRACT

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.

15.
Nanomaterials (Basel) ; 12(15)2022 Aug 07.
Article in English | MEDLINE | ID: mdl-35957144

ABSTRACT

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.

16.
Micromachines (Basel) ; 13(8)2022 Aug 21.
Article in English | MEDLINE | ID: mdl-36014283

ABSTRACT

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.

17.
Microsc Res Tech ; 85(11): 3633-3641, 2022 Nov.
Article in English | MEDLINE | ID: mdl-35916245

ABSTRACT

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.


Subject(s)
Oils, Volatile , Fractals , Gelatin , Microscopy, Atomic Force , Polymers , Surface Properties
18.
Materials (Basel) ; 15(15)2022 Aug 05.
Article in English | MEDLINE | ID: mdl-35955350

ABSTRACT

Considerable efforts have been spent on environmentally friendly particles for the encapsulation of essential oils. Polymeric particles were developed to encapsulate the essential oil from Piper nigrum based on gelatin and poly-ε-caprolactone (PCL) carriers. Gas Chromatography ((Flame Ionization Detection (GC/FID) and Mass Spectrometry (GC/MS)), Atomic Force Microscopy (AFM), Nanoparticle Tracking Analysis (NTA), Confocal Laser Scanning Microscopy (CLSM), Attenuated Total Reflectance-Fourier-transform Infrared Spectroscopy (ATR-FTIR), and Ultraviolet-Visible (UV-VIS) spectroscopy were used for the full colloidal system characterization. The essential oil was mainly composed of ß-caryophyllene (~35%). The stability of the encapsulated systems was evaluated by Encapsulation Efficiency (EE%), electrical conductivity, turbidity, pH, and organoleptic properties (color and odor) after adding different preservatives. The mixture of phenoxyethanol/isotialzoni-3-one (PNE system) resulted in enhanced stability of approximately 120 and 210 days under constant handling and shelf-life tests, respectively. The developed polymeric system presented a similar controlled release in acidic, neutral, or basic pH, and the release curves suggested a pulsatile release mechanism due to a complexation of essential oil in the PCL matrix. Our results showed that the developed system has potential as an alternative stable product and as a controlling agent, due to the pronounced bioactivity of the encapsulated essential oil.

19.
Sci Rep ; 12(1): 12002, 2022 Jul 14.
Article in English | MEDLINE | ID: mdl-35835814

ABSTRACT

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.

20.
Molecules ; 27(12)2022 Jun 08.
Article in English | MEDLINE | ID: mdl-35744819

ABSTRACT

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.


Subject(s)
Hot Temperature , Polyamines , Aniline Compounds , Electric Conductivity , Poly A , Polyamines/chemistry , Polymers/chemistry
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