Morpho-structural Properties Research Articles

TiO2 aerogel − A sensing electrode matrix for the sensitive detection of diclofenac sodium

This study developed a new composite matrix containing TiO2 aerogel having mesoporous structure (TiO2AG), bioengineered flagellin (bioF) and chitosan (Ch) deposited on a glassy carbon electrode (GCE), for the detection of diclofenac sodium (DS) in aqueous solutions. It is worth mentioning that TiO2AG mesoporous material was used for the first time as a sensitive matrix for DS detection. The morpho-structural properties of the new electrode materials were assessed by X-ray diffraction (XRD), N2 adsorption–desorption measurements, and scanning electron microscopy (SEM) in conjunction with energy-dispersive X-ray spectroscopy. The electrochemical properties of the new bioF + TiO2AG + Ch/GCE modified electrode were determined by cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS) and square wave voltammetry (SWV) techniques. The developed modified electrode exhibits a significant electrocatalytic activity for DS electrooxidation process reflected in the acquired performances (detection limit of 17 nM, sensitivity of 0.41 A/M, linear range from 0.15 to 2.5 µM), and presents excellent reproducibility, repeatability, and stability. The practical use of the new developed electrode was estimated by quantifying DS in pharmaceutical formulations (recovery mean of 100.66 % for DS, with a relative standard deviation of 0.39 %) and wastewater samples (relative error of 3.15 % and a relative standard deviation of 0.393 when compared to the LC-MS standard technique).

Insight into Romanian Wild-Grown Heracleum sphondylium: Development of a New Phytocarrier Based on Silver Nanoparticles with Antioxidant, Antimicrobial and Cytotoxicity Potential.

Background: Heracleum sphondylium, a medicinal plant used in Romanian ethnopharmacology, has been proven to have remarkable biological activity. The escalating concerns surrounding antimicrobial resistance led to a special attention being paid to new efficient antimicrobial agents based on medicinal plants and nanotechnology. We report the preparation of a novel, simple phytocarrier that harnesses the bioactive properties of H. sphondylium and silver nanoparticles (HS-Ag system). Methods: H. sphondylium's low metabolic profile was determined through gas chromatography-mass spectrometry and electrospray ionization-quadrupole time-of-flight-mass spectrometry. The morphostructural properties of the innovative phytocarrier were analyzed by X-ray diffraction, Fourier-transform infrared spectroscopy, Raman spectroscopy, dynamic light scattering, scanning electron microscopy, and energy-dispersive X-ray spectroscopy. The antioxidant activity was evaluated using total phenolic content, ferric reducing antioxidant power, and 2,2-diphenyl-1-picrylhydrazyl (DPPH) in vitro assays. The antimicrobial activity screening against Staphylococcus aureus, Bacillus subtilis, Pseudomonas aeruginosa, and Escherichia coli was conducted using the agar well diffusion method. The 3-(4,5-Dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide (MTT) assay estimated the in vitro potential cytotoxicity on normal human dermal fibroblasts (NHDF) and cervical cancer (HeLa) cells. Results: A total of 88 biomolecules were detected, such as terpenoids, flavonoids, phenolic acids, coumarins, phenylpropanoids, iridoids, amino acids, phytosterols, fatty acids. The HS-Ag phytocarrier heightened efficacy in suppressing the growth of all tested bacterial strains compared to H. sphondylium and exhibited a significant inhibition of HeLa cell viability. Conclusions: The new HS-Ag phytocarrier system holds promise for a wide range of medical applications. The data confirm the capacity to augment the pertinent theoretical understanding in the innovative field of antimicrobial agents.

Raw clay material-based modified carbon paste electrodes for sensitive heavy metal detection in drinking water

A new electrode based on carbon paste (CP) modified with natural clay was used for heavy metals detection. The investigation of the raw clay material (X-ray diffraction, infrared spectroscopy, scanning electron microscopy, energy-dispersive X-ray spectroscopy, thermal analysis and particle size distribution) revealed different morpho-structural properties of the natural material. The electrochemical behaviour of the modified carbon paste electrode and its ability to detect heavy metals (Zn2+, Cd2+, and Cu2+) was studied by different electrochemical techniques like cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS), and square wave anodic stripping voltammetry (SWASV). Both electrochemical and analytical parameters of the investigated modified electrode recommend them as stable, sensitive and reproducible sensors for individual heavy metals detection.

Obtaining and characterization of doped lanthanum manganite through an unconventional method

Considering the growing concern for food safety, the development of fast detection methods with high sensitivity and repeatability of specific food constituents is a huge necessity. In this regard, the electrochemical methods can be an effective way due to certain advantages such as low cost, fast response signal, high sensitivity and ease of use. The detection efficiency of electrochemical sensors mainly depends on the electrochemical characteristics of the electrode materials. Perovskite-based materials are ideal candidates for the development of electrochemical sensors due to their excellent catalytic activity and redox properties. We report herein the synthesis, morpho-structural properties, and electrical performance assessment of Ca doped lanthanum manganite by ultrasonic method with immersed sonotrode in the reaction medium. X-ray diffraction (XRD) and scanning electron microscopy (SEM) analyses were performed on the synthesized samples. The results indicated a wellcrystallized perovskite-type structure, and 29 nm average crystallite sizes. The electron microscopy images showed that the presence of the dopant influenced the surface morphology.

Advancements in polyol synthesis: expanding chemical horizons and Néel temperature tuning of CoO nanoparticles

The polyol synthesis of CoO nanoparticles (NPs) is typically conducted by dissolving and heating cobalt acetate tetrahydrate and water in diethylene glycol (DEG). This process yields aggregates of approximately 100 nm made of partially aligned primary crystals. However, the synthesis demands careful temperature control to allow the nucleation of CoO while simultaneously preventing reduction, caused by the activity of DEG. This restriction hinders the flexibility to freely adjust synthesis conditions, impeding the ability to obtain particles with varied morpho-structural properties, which, in turn, directly impact chemical and physical attributes. In this context, the growth of CoO NPs in polyol was studied focusing on the effect of the polyol chain length and the synthesis temperature at two different water/cations ratios. During this investigation, we found that longer polyol chains remove the previous limits of the method, allowing the tuning of aggregate size (20–150 nm), shape (spherical-octahedral), and crystalline length (8–35 nm). Regarding the characterization, our focus revolved around investigating the magnetic properties inherent in the synthesized products. From this point of view, two pivotal findings emerged. Firstly, we identified small quantities of a layered hydroxide ferromagnetic intermediate, which acted as interference in our measurements. This intermediate exhibited magnetic properties consistent with features observed in other publications on CoO produced in systems compatible with the intermediate formation. Optimal synthetic conditions that prevent the impurity from forming were found. This resolution clarifies several ambiguities existing in literature about CoO low-temperature magnetic behavior. Secondly, a regular relationship of the NPs' TN with their crystallite size was found, allowing us to regulate TN over ~ 80 K. For the first time, a branching was found in this structure-dependent magnetic feature, with samples of spheroidal morphology consistently having lower magnetic temperatures, when compared to samples with faceted/octahedral shape, providing compelling evidence for a novel physical parameter influencing the TN of a material. These two findings contribute to the understanding of the fundamental properties of CoO and antiferromagnetic materials.

Morphostructural studies of pure and mixed metal oxide nanoparticles of Cu with Ni and Zn

Nano-scale interactions between pure metal or metal-oxide components within an oxide matrix can improve functional performance over basic metal oxides. This study reports on the synthesis of monometallic (CuO), bimetallic (CuO–NiO) and trimetallic (CuO–NiO–ZnO) oxide nanoparticles (NPs) via the co-precipitation method and investigation of morphostructural properties. All of the synthesized metal oxide NPs were calcined at 550 °C temperature and annealed under vacuum. In this work, we applied Scherrer formula, modified Scherrer equation, Williamson-Hall plots, and Halder-Wagner plots to calculate the average crystallite size. The XRD data analysis showed that average crystallite sizes of the as-synthesized metal oxide phases were between 4 nm and 76 nm and average diameters calculated from SEM image were between 15 nm and 83 nm. The XRD studies also disclosed that average crystallite size and lattice microstrain of the CuO phases remain almost same (43 nm–46 nm and 2.074×10−3 to 2.665×10−3) for pure CuO and mixed CuO–NiO; but in case of mixed CuO–NiO–ZnO it is found to decrease in size to 11 nm where lattice microstrain increases to 9.653×10−3. Line broadening of diffraction peaks from microstrain contribution was between 0.02 and 0.01. Degree of crystallinity (%) of CuO phases found to decrease from 81 to 71. Dislocation density of CuO phases found to increase from 6.63×10−4nm−2 to 12.68×10−3nm−2. X-ray density of CuO phases increased from 6.48 to 6.53 g/cm3. Where this calculated small dislocation density well agreed with the high crystallinity. Crystal structure and specific surface area were determined from lattice constants and X-ray density. These synthesized nanopowders showed the existence of monoclinic, cubic, and hexagonal phases. The obtained NPs of multi-metal oxide explained more than one phases with different size, shape, and morphology at nano scale.

Evaluation of the Bioenergy Potential of Blends (Green Coconut Shells and Fish Scales) as a Feedstock in Thermochemical Processes for Clean Energy Production

Brazil is among the world’s largest producers of green coconut, which contributes to inappropriate disposal and socioenvironmental impacts. Concomitantly, some of its coastal cities produce a great diversity of fish and large amounts of solid waste. This paper reports on the use of samples of fish scales (100FS) and green coconut shells (100GCS) and their mixtures in 75%FS:25%GCS (B25), 50%FS:50%GCS (B50), and 25%FS:75%GCS (B75) proportions and quantification of their Higher Heating Values (HHV) and Lower Heating Values (LHV), and Ultimate (UA) and Proximate Analyses (PA). Their thermal behavior was investigated by thermogravimetry (TG/DTG) and differential scanning calorimetry (DSC), whereas scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), X-ray diffraction (XRD), and Fourier transformed infrared (FTIR) were employed for analyses of their physicochemical and morphostructural properties. When compared to in natura samples, SEM images of the blends detected a structural disorder and a highly fibrous structure with an elongated chain and surface roughness. HHV were superior in samples with 100GCS (16.64 MJ kg−1), B75 (15.80 MJ kg−1), and B50 (14.98 MJ kg−1), and lower in B25 (14.16 MJ kg−1) and 100FS (13.03 MJ kg−1), with acceptable values for different biomasses. TG/DTG and DSC curves showed similarities among the samples, with the detection of their main thermoconversion stages. According to the data, the samples can be applied as renewable energy sources to mitigate socioecological illnesses and social vulnerabilities resulting from the archaic and inadequate management of solid waste.

Investigation of wet etching technique for selective patterning of ferroelectric zirconium-doped hafnium oxide thin films for high-frequency electronic applications

This paper presents the area-selective wet etching (ASWE) method as a novel approach to have a selective patterning of a 6.8 nm-thick zirconium-doped hafnium oxide (HZO) thin film, to improve the performance of a metal ferroelectric metal (MFM)-like structure. According to the electromagnetic simulations of microwave phase shifters with patterned HZO thin films, it is underlined the importance to have selectively targeted areas covered with HZO instead of full-coverage wafers, to gain a further increase in the microwave performance of low-voltage tunable high-frequency components. The impact of the ASWE method on the morpho-structural properties was studied using various investigation tools in a non-destructive manner. X-ray reflectivity (XRR) has been employed at different immersion times, up to 120 s. Based on the extended Fast Fourier Transform (FFT) analysis, as well as from the simulation of the experimental curves in the framework of parallel-tempering algorithm, the determination of the etching rate became possible. X-ray diffraction (XRD), atomic force microscopy (AFM), and X-ray photoelectron spectroscopy (XPS) clearly indicated the complete removal of HZO after etching processes at 180 s. The method is fast, reliable, and low-cost, thus filling the actual gap in providing the necessary ferroelectric thin films exclusively in selected areas of interest.

Engineering the Morphostructural Properties and Drug Loading Degree of Organic-Inorganic Fluorouracil-MgAl LDH Nanohybrids by Rational Control of Hydrothermal Treatment.

Layered double hydroxides (LDHs) or hydrotalcite-like compounds have attracted great attention for the delivery of anticancer drugs due to their 2D structure, exhibiting a high surface-to-volume ratio and a high chemical versatility. The drug is protected between the layers from which it is slowly released, thus increasing the therapeutic effect and minimizing the side effects associated to nonspecific targeting. This work aimed to design LDHs with Mg and Al (molar ratio of 2/1) in brucite-like layers, which retained fluorouracil (5-FU; 5-FU/Al = 1, molar ratio) in the interlayer gallery as the layers grow during the co-precipitation step of the synthesis. To rationally control the physicochemical properties, particularly the size of the crystallites, the aging step following the co-precipitation was performed under carefully controlled conditions by changing the time and temperature (i.e., 25 °C for 16 h, 100 °C for 16 h, and 120 °C for 24 h). The results revealed the achievement of the control of the size of the crystals, which are gathered in three different agglomeration systems, from tight to loose, as well as the loading degree of the drug in the final organic-inorganic hybrid nanomaterials. The role played by the factors and parameters affecting the drug-controlled release was highlighted by assessing the release behavior of 5-FU by changing the pH, solid mass/volume ratio, and ionic strength. The results showed a pH-dependent behavior but not necessarily in a direct proportionality. After a certain limit, the mass of the solid diminishes the rate of release, whereas the ionic strength is essential for the payload discharge.

Romanian Wild-Growing Armoracia rusticana L.-Untargeted Low-Molecular Metabolomic Approach to a Potential Antitumoral Phyto-Carrier System Based on Kaolinite.

Horseradish is a globally well-known and appreciated medicinal and aromatic plant. The health benefits of this plant have been appreciated in traditional European medicine since ancient times. Various studies have investigated the remarkable phytotherapeutic properties of horseradish and its aromatic profile. However, relatively few studies have been conducted on Romanian horseradish, and they mainly refer to the ethnomedicinal or dietary uses of the plant. This study reports the first complete low-molecular-weight metabolite profile of Romanian wild-grown horseradish. A total of ninety metabolites were identified in mass spectra (MS)-positive mode from nine secondary metabolite categories (glucosilates, fatty acids, isothiocyanates, amino acids, phenolic acids, flavonoids, terpenoids, coumarins, and miscellaneous). In addition, the biological activity of each class of phytoconstituents was discussed. Furthermore, the development of a simple target phyto-carrier system that collectively exploits the bioactive properties of horseradish and kaolinite is reported. An extensive characterization (FT-IR, XRD, DLS, SEM, EDS, and zeta potential) was performed to investigate the morpho-structural properties of this new phyto-carrier system. The antioxidant activity was evaluated using a combination of three in vitro, non-competitive methods (total phenolic assay, 2,2-Diphenyl-1-picrylhydrazyl (DPPH) radical-scavenging assay, and phosphomolybdate (total antioxidant capacity)). The antioxidant assessment indicated the stronger antioxidant properties of the new phyto-carrier system compared with its components (horseradish and kaolinite). The collective results are relevant to the theoretical development of novel antioxidant agent fields with potential applications on antitumoral therapeutic platforms.

Effect of Urea as a Shape-Controlling Agent on the Properties of Bismuth Oxybromides

Bismuth oxybromides were prepared via a solvothermal method by applying different urea amounts during synthesis. The effects of the urea ratio on the morpho–structural properties and photocatalytic activity of the samples were investigated. X-ray diffraction, diffuse reflectance spectroscopy, infrared spectroscopy, Raman spectroscopy, scanning electron microscopy, and surface tension measurements were carried out to characterize the samples. Their photoactivity was evaluated by the photocatalytic degradation of rhodamine B and ibuprofen under UV and visible light irradiations. The urea ratio notably influenced morphology, particle size distribution, and photoactivity. However, it only had a limited effect on the crystalline composition, primary crystallite size, and band gap of bismuth oxybromides. The formation of Bi-based complexes and degraded urea-based products were observed, which were deduced to influence band gap energies and hence, photoactivity. Predominantly, samples prepared at low urea ratios proved to be the best for both rhodamine B and ibuprofen degradations under both irradiations.

Effects of drying conditions and ethanol pretreatment on the techno-functional and morpho-structural properties of avocado powder produced by foam-mat drying

Effects of drying conditions and ethanol pretreatment on the techno-functional and morpho-structural properties of avocado powder produced by foam-mat drying

Modification of Cotton and Leather Surfaces Using Cold Atmospheric Pressure Plasma and TiO2-SiO2-Reduced Graphene Oxide Nanopowders

Surface modification of textile fabrics and leathers is very versatile and allows the products quality improvement. In this work, cotton and leather substrates were pre-treated with cold atmospheric pressure plasma (CAPP) and further coated with TiO2-SiO2-reduced graphene oxide composites in dispersion form. By using a Taguchi scheme, this research evaluated the effect of three significant parameters, i.e., the pre-treatment with CAPP, organic dispersion coating and TiO2-SiO2-reduced graphene oxide (TS/GR) composites, that may affect the morpho-structural properties and photocatalytic activity of modified cotton and leather surfaces. The characteristics of cotton/leather surfaces were evaluated by morphological, structural, optical and self-cleaning ability using scanning electron microscopy with energy dispersive X-ray spectroscopy (SEM/EDX), X-ray powder diffraction (XRD), attenuated total reflection-Fourier Transform Infrared spectroscopy (ATR-FTIR) and UV-Vis spectroscopy. The self-cleaning performance of the obtained cotton and leather samples was evaluated by photocatalytic discoloration of berry juice surface stains under UV light irradiation for 12 h. The successfulness of coating formulations was proven by the SEM analysis and UV-Vis spectroscopy. The XRD patterns and ATR-FTIR spectra revealed the cellulose and collagen structures as dominant components of cotton and leather substrates. The CAPP treatment did not damage the cotton and leather structures. The photocatalytic results highlighted the potential of TiO2-SiO2-reduced graphene oxide composites in organic dispersion media, as coating formulations, for further use in the fabrication of innovative self-cleaning photocatalytic cotton and leather products.

The influence of the synthesis method on Gd2O3 morpho-structural properties and sensitivity to CO2 under in-field conditions

In this study, we report the implications of the synthesis method on Gd2O3 sensitivity to CO2. The rare-earth oxide was prepared by wet chemical co-precipitation and by hydrothermal method. The obtained powders labelled Gd2O3–CoP and Gd2O3-HT were deposited as thick films over commercial Al2O3 substrates provided with Pt electrodes and a back-side heater. Both powders consist of the same crystallographic phase, with a significant difference appearing in selected area electron diffraction patterns, transmission electron microscopy images at higher magnification and X-ray diffraction spectra, with respect to the crystallization degree. The associated role in sensing properties is revealed via electrical resistance variations determined by CO2 concentrations in the range between 400 and 3000 ppm and variable relative humidity between 0 and 50%RH, similar to the in-field atmosphere. The proposed CO2 interaction mechanism is based on phenomenological investigations which highlight the electronic affinity variation as the effect of dipoles induced by the in-field conditions on the Gd2O3 surface.

Study of the Synthetic Approach Influence in Ni/CeO2-Based Catalysts for Methane Dry Reforming

This study focuses on the synthetic approach influence in morphostructural features and catalytic performances for Ni/CeO2 catalysts. Incipient wetness impregnation, coprecipitation and nitrate combustion were studied as catalyst preparation approaches, and the materials were then tested at 700 °C for methane dry reforming (MDR). The morphostructural properties of the materials were deeply studied using several techniques, such as temperature programmed reduction (TPR), to investigate reducibility and support-metal interaction, N2 physisorption to evaluate the porosity and the surface area, scanning electron microscopy (SEM) and X-ray diffraction (XRD) to estimate Ni dispersion, and temperature programmed oxidation (TPO) to identify the type and amount of coke formed on catalysts’ surface after reaction. From the data obtained, coprecipitation turned out to be the most suitable technique for this application because this catalyst was able to reach 70% of CO2 conversion and 30% methane conversion, with an H2 yield of 15% and 30% yield of CO at the end of the 30 h test. Moreover, it was also the catalyst with the highest metal dispersion, the strongest interaction with the support, and the lowest coke deposition.

Untargeted Metabolomic Approach of Curcuma longa to Neurodegenerative Phytocarrier System Based on Silver Nanoparticles.

Curcuma is one of the most famous medicinal and tropical aromatic plants. Its health benefits have been appreciated and exploited in traditional Asian medicine since ancient times. Various studies have investigated its complex chemical composition and demonstrated the remarkable therapeutic properties of curcuma's phytoconstituents. Oxidative stress is a decisive driving factor triggering numerous pathologies (neurodegenerative, psychiatric and cardiovascular diseases; diabetes; tumors, etc.). Numerous recent studies have focused on the use of natural compounds and nanomaterials as innovative molecular targeting agents as effective therapeutic strategies. In this study, we report, for the first time, the development of a simple target phytocarrier system that capitalizes on the bioactive properties of curcuma and AgNPs. The complete metabolic profile of curcuma was determined based on gas chromatography-mass spectrometry (GC-MS) and electrospray ionization quadrupole time-of-flight mass spectrometry (ESI-QTOF-MS). A total of 80 metabolites were identified under mass spectra (MS)-positive mode from 10 secondary metabolite categories: terpenoids, amino acids, diarylheptanoids, flavonoids, phenolic acids, steroids, fatty acids, coumarins, alkaloids and miscellaneous. In addition, the biological activity of each class of metabolites was discussed. A comprehensive characterization (FT-IR, UV-Vis, DLS, SEM, TEM, EDS, zeta potential and XRD) was performed to study the morphostructural properties of this new phytocarrier system. Antioxidant activity of the new phytocarrier system was evaluated using a combination of in vitro methods (total phenolic assay, 2,2-Diphenyl-1-picrylhydrazyl (DPPH) radical scavenging assay and cyclic voltammetric method (Trolox equivalent antioxidant capacity (TEAC) electrochemical assay)). Antioxidants assays showed that the phytocarrier system exhibits superior antioxidant properties to those of its components, i.e., curcuma or citrate-coated-AgNPs. These data confirm the potential to enhance relevant theoretical knowledge in the area of innovative antioxidant agents, with potential application in neurodegenerative therapeutic strategies.

Investigation on the coacervation of fish scale gelatin hydrogel with seafood waste hydrolysates for the development of artificial fish bait: Physico-chemical, thermodynamic, and morpho-structural properties

The study dealt with the development of biopolymer based hydrogel artificial fish bait with hydrolysates derived from fish processing wastes. Fish scale gelatin (FSG) was used for the development of a hydrogel to which bioattractants extracted from seafood processing wastes of fish, squid and shrimp were added to prepare composite gels such as FSG-FH, FSG-SH and FSG-SPH, respectively. To understand the homogenesity and cross linking complexation of composite gels, the study aimed at investigating physico-chemical, thermodynamic, molecular and structural properties were analysed. The gel strength, melting point and thermal stability of the composite hydrogels were found to decrease marginally compared to the control gel, FSG. It could be understood that the crystalline structure at 2θ = 23° of the FSG-SH, and FSG-FH were not much altered compared to FSG gel. However, alteration in the crystalline structure in FSG-SPH was evident at 2θ = 27.3°. The TGA and DSC analysis revealed the reduction in the thermal stability of FSG on the addition of protein hydrolysates in the process of coacervation to get hydrogel based fish bait. Further, FESEM and AFM analysis indicated FSG-SH as the composite hydrogel with most compact and smooth surface was evident by Ra and Rq values. Among the composite gels, FSG-SH was found to have higher hydrophobicity due to enhanced gel structure. FTIR spectra of FSG and composite gels exhibitted similarity corresponding to amide-A, B, I, II and III bands. However, NMR analysis revealed the existence of notable difference with respect to chemical shift in the range of 7.0–7.75 ppm expressing the presence of aromatic protons of the amino acid phe and N–H protons of amide in all the composite gels. Further, NMR analysis confirmed the role of imino acids (δ CH2 & β CH2 protons) and hydrophobic amino acids (α-CH2 protons) in decrease the physical and thermal properties of the composite gels. The addition of protein hydrolysates with FSG was found to decrease the physical, thermal and structural properties, however improve the aromatic compounds of the composite gels.

Structural and Magnetic Specificities of Fe-B Thin Films Obtained by Thermionic Vacuum Arc and Magnetron Sputtering

Fe-B based compounds are of high interest due to their special properties and the wide range of involved applications. While B is the element that facilitates the increase in the hardness and the degree of wear resistance, it is also an effective glass former, controlling the formation of a much-desired amorphous structure with specific magnetic properties. Major difficulties related to the proper engineering of Fe-B thin films lay especially in their preparation under well-defined compositions, which in turn, should be accurately determined. The present study closely analyzes the morpho-structural and magnetic properties of thin coatings of Fe-B of approximately 100 nm thickness and with the nominal B content ranging from 5 at. % to 50 at. %. The comparison between films obtained by two preparation methods, namely, the thermionic vacuum arc and the magnetron sputtering is envisaged. Morpho-structural properties were highlighted using X-ray diffraction supplemented with X-ray reflectometry and scanning electron microscopy, whereas the elemental investigations were performed by X-ray dispersive spectroscopy and Rutherford back-scattering spectroscopy. The magnetic properties of the Fe-B layers were carefully investigated by the vectorial magneto-optic Kerr effect and conversion electron Mössbauer spectroscopy. The high capability of Mössbauer Spectroscopy to provide the phase composition and the B content in the formed Fe-B intermetallic films was proven, in correlation to Rutherford back-scattering techniques, and to explain their magnetic properties, including the magnetic texture of interest in many applications, in correlation with longitudinal magneto-optic-Kerr-effect-based techniques.

The impact of the synthesis temperature on SnO2 morphology and sensitivity to CO2 under in-field conditions

The impact of the synthesis temperature on SnO 2 morphology and sensitivity to CO 2 under in-field conditions • SnO 2 is obtained by hydrothermal method, at different synthesis temperatures. • SnO 2 crystalline nanoparticles are faceted, with regular morphologies. • Main crystallographic planes (0 0 1), (1 0 1), (1 1 0) contain oxygen positions. • The sensing properties are evaluated under in-field conditions, RH = 0–50 %. • CO 2 concentration varies between 400 and 5000 ppm CO 2 . This letter highlights the role of synthesis temperature over the morpho-structural properties of SnO 2 . Specific crystalline nanoparticles with quasi-tetragonal and quasi-hexagonal morphologies are faceted, suggesting a high reactivity to atmospheric oxygen. This is a premise for the sensing ability of SnO 2 in detecting CO 2 . The in-field conditions are ensured by dynamic synthetic air flow with variable relative humidity, a wide range of CO 2 concentrations and potential interfering gases at their specific detection limits.

Effect of enzymatic hydrolysis on digestibility and morpho-structural properties of hydrothermally pre-treated red rice starch

The objective of this work was to evaluate the effects of enzymatic hydrolysis on digestibility and morphological and structural properties of hydrothermally pre-treated (HPT) red rice starch. The pre-treatments were performed in autoclave and cooking for the modification of rice grains and native starch. In vitro starch digestibility was performed consecutively and semi-simultaneously using α-amylase and amyloglucosidase. A first-order mathematical model was used to adjust the hydrolysis kinetic data, which made it possible to calculate the surface area, hydrolysis index, and glycemic index of the starch. Scanning electron microscopy images (SEM), Fourier transform infrared (FTIR) spectra and X-ray diffraction (XRD) were also performed to investigate the characteristics of the post-hydrolysis starch samples. The autoclaved starch HSS-A3, which was subjected to 121 °C/1.08 bar for 10 min, showed the highest in vitro digestibility values (80.08 %). Both starch samples showed increase of particle size and enzymatic digestibility after HPT. FTIR spectra of the starch samples showed that there was no appearance of new functional groups. However, XRD evidenced that HPT changed the intensity of the peaks and the type of crystallinity was changed for autoclaved starch (A3) from type A to Vh, with crystallinity ranging from 21.71 % to 26.42 %. The semi-simultaneous approach showed more advantages due to the highest in vitro digestibility as well as reducing the processing time and use of reagents.