Atomic Force Microscopy Techniques Research Articles

Macroscopic and microscopic investigations of determining elasto-mechanical properties of limequat fruit.

Given the paramount importance of agricultural products in global health and food security, and the increasing consumer demand, understanding the mechanical behavior of these materials under various conditions is necessary yet challenging. Due to their heterogeneous and non-uniform nature, determining their mechanical behavior is complex. This study employs atomic force microscopy (AFM) to determine the modulus of elasticity of limequat fruit at the microscopic scale and compares it with macroscopic methods. The analyses revealed a statistically significant difference (at the 1% level) in the mechanical behavior determined at the macroscopic scale. The highest modulus of elasticity, 0.752 MPa, was observed using Hertz's theory under complete placement between two parallel planes. The lowest, 0.059 MPa, was noted when a spherical probe compressed a rectangular sample. The average modulus of elasticity of the limequat peel was 2.007 MPa. At the microscopic scale, the modulus of elasticity of the fruit tissue ranged from 0.370 to 0.365 MPa, and for the peel, it was 0.246 MPa. RESEARCH HIGHLIGHTS: Working principles of this innovative technique were elaborated. The AFM technique used provide elasto-mechanical properties determination of cell walls of single living cells extracted from biological materials on the nanoscale. By combining AFM topographical image and nano-indentation of living fruit cells it will be possible to investigate cells' elasto-mechanical properties. Atomic force microscopy holds great potential for monitoring fruit mechanical properties of biological materials.

B-064 Bovine Serum Albumin Coats Silicon Dioxide More Uniformly Near its Isoelectric Point Based on Atomic Force Microscopy Analysis

Abstract Background Bovine serum albumin (BSA) serves as a blocking agent in in-vitro diagnostic (IVD) applications, with fatty acid stabilized (FAS) and fatty acid free (FAF) BSA as common options. The presence of fatty acids and pH influence the conformation of BSA. While previous studies have explored the individual effects of fatty acids or pH on BSA blocking, limited data exists on their combined impact. This study employs atomic force microscopy (AFM) to investigate how pH and fatty acids jointly affect BSA adsorption onto silica, a surface relevant within diagnostics. Methods AFM, a sensitive microscopic technique, provides topographic images of surfaces with superior resolution compared to optical microscopy. We conducted experiments to assess the adsorption of 1% FAS and FAF BSA on a silica surface at pH 5.2 and pH 7. Evaluation of the coatings involved scratching to assess overall thickness, and roughness, indicating thickness variability. Results Results revealed that both fatty acids and pH play significant roles in shaping the BSA coating characteristics on silica surfaces. In three out of four experimental conditions, the average thickness of the BSA coating ranged between 3-4 nm, except for FAS BSA at pH 7, which exhibited a thicker average coating measuring 5.6 nm. The pH impacted the roughness of the BSA coating. Coatings prepared at pH 5.2 displayed smoother surfaces compared to those at pH 7. Utilizing the root mean square average height variability analysis, there is 95% confidence that the FAF and FAS BSA surfaces at pH 5.2 had a height range between 2.4-4.3 nm and 2.0-4.9 nm, respectively, indicating complete coverage of the silica surface without much height variation. In contrast, the FAF and FAS BSA coatings at pH 7 exhibited a wider range of heights, with 95% confidence intervals spanning from -1.5-8.6 nm and 0.0-11.2 nm, respectively. This variability suggests potential issues including incomplete BSA coverage at the lower range, and steric hindrance at the higher end, highlighting the importance of pH in optimizing BSA coatings for various applications. Conclusions Silica is commonly used in IVD assays, with BSA frequently employed to coat and passivate the surface. Our AFM experiments highlight the impact of pH and fatty acid presence on coating thickness and uniformity. Notably, FAS BSA at pH 7 exhibited the thickest coating; however, its increased roughness may pose challenges in IVD applications due to steric hindrance blocking antibody-antigen interactions. Alternatively, FAF BSA at pH 7 displayed an adequate thickness but also considerable roughness, suggesting potential insufficiencies in surface coverage and passivation. FAS and FAF BSA coatings at pH 5.2 showed relatively consistent thickness, indicating a more uniform surface which may be ideal for IVD coating applications. These AFM experiments were conducted on pure silica surfaces, which may differ from surfaces engineered for IVD. Additionally, both FAF and FAS BSA grades are proven to be effective in IVD applications. Further research employing AFM and other biophysical techniques is warranted to deepen our understanding of pH and fatty acid effects on BSA-surface interactions, aiming to enhance blocking strategies in IVD.

Applying the Atomic Force Microscopy Technique in Medical Sciences-A Narrative Review.

Penetrating deep into the cells of the human body in real time has become increasingly possible with the implementation of modern technologies in medicine. Atomic force microscopy (AFM) enables the effective live imaging of cellular and molecular structures of biological samples (such as cells surfaces, components of biological membranes, cell nuclei, actin networks, proteins, and DNA) and provides three-dimensional surface visualization (in X-, Y-, and Z-planes). Furthermore, the AFM technique enables the study of the mechanical, electrical, and magnetic properties of cells and cell organelles and the measurements of interaction forces between biomolecules. The technique has found wide application in cancer research. With the use of AFM, it is not only possible to differentiate between healthy and cancerous cells, but also to distinguish between the stages of cancerous conditions. For many years, AFM has been an important tool for the study of neurodegenerative diseases associated with the deposition of peptide amyloid plaques. In recent years, a significant amount of research has been conducted on the application of AFM in the evaluation of connective tissue cell mechanics. This review aims to provide the spectrum of the most important applications of the AFM technique in medicine to date.

Investigation of PVDF‐co‐HPF based ultrafiltration polymer inclusion membrane for the extraction of cadmium ions

AbstractUltrafiltration polymer inclusion membranes (UPIMs) have become increasingly significant for the separation and purification of heavy metals from industrial wastes and wastewater due to their convenience compared to other liquid membranes. A novel process for cadmium separation and recovery has been developed using biodegradable ion carriers, specifically room temperature ionic liquids with various molecular structures. This innovation has greatly enhanced the efficiency and application of UPIMs for cadmium separation, while also providing the membranes with unique functional properties. In this study, various UPIMs were produced using polyvinyl fluoride hexafluoropropylene (PVDF‐co‐HPF) as the base polymer, different plasticizers, and symmetric room temperature ionic liquids as ion carriers. The ability of these membranes to extract cadmium ions was evaluated, demonstrating a removal rate of 9.70 μmol s−1 from a 25 ppm Cd(II) solution under optimum conditions. The selectivity and stability of the optimized UPIM were examined under different conditions to obtain a deeper insight into of its performance. The morphological characteristics of the optimized UPIM were examined using scanning electron microscopy and atomic force microscopy techniques.

Cell surface morphology mimicking nano-bio platform for immune cell stimulation

Studying the complex realm of cellular communication and interactions by fluorescence microscopy requires sample fixation on a transparent substrate. To activate T cells, which are pivotal in controlling the immune system, it is important to present the activating antigen in a spatial arrangement similar to the nature of the antigen-presenting cell, including the presence of ligands on microvilli. Similar arrangement is predicted for some other immune cells. In this work, immune cell-stimulating platform based on nanoparticle-ligand conjugates have been developed using a scalable, affordable, and broadly applicable technology, which can be readily deployed without the need for state-of-the-art nanofabrication instruments. The validation of surface biofunctionalization was performed by combination of fluorescence and atomic force microscopy techniques. We demonstrate that the targeted system serves as a biomimetic scaffold on which immune cells make primary contact with the microvilli-mimicking substrate and exhibit stimulus-specific activation.

Probing the interactions between asphaltenes and a PEO-PPO demulsifier at oil–water interface: Effect of temperature

HypothesisAsphaltenes are primary stabilizers in water-in-oil (W/O) emulsions that cause corrosion and fouling issues. In oilsands industry, oil/water separation processes are generally conducted at high temperatures. A high temperature is expected to impact the interactions between asphaltenes and emulsion breakers (EBs), consequently influencing demulsification performance. ExperimentsThe adsorption and interactions of asphaltenes and a PEO-PPO type EB (Pluronic F68) at the oil–water interface were investigated at various temperatures, using tensiometer, quartz crystal microbalance with energy dissipation (QCM-D), and atomic force microscopy (AFM). The effect of temperature on EB’s demulsification performance was explored through bottle tests. Additionally, demulsification mechanisms were studied using direct force measurements with the droplet probe AFM technique. FindingsDynamic interfacial tension and QCM-D results demonstrate that the PEO-PPO type EB exhibits higher interface activity than asphaltenes and can disrupt rigid asphaltene films at the oil–water interface. Elevated temperatures accelerate the displacement of adsorbed asphaltenes by EB molecules, leading to sparse interfacial films and rapid droplet coalescence (supported by AFM results). This work provides valuable insights into interfacial interactions between asphaltenes and EB under different temperatures, enhancing the understanding of demulsification mechanisms and offering useful implications for the development of efficient EBs to enhance oil/water separation performance.

Laser engineered architectures for magnetic flux manipulation on superconducting Nb thin films

Custom shaped magnetic flux guiding channels have been fabricated on superconducting Nb thin films by laser nanopatterning of their surface. Preferential pathways are defined by suitable combination of imprinted anisotropic pinning domains through laser-induced periodic surface structures (LIPSS). Generated by the selective energy deposition of femtosecond UV laser pulses, quasi-parallel ripple structures are formed under optimized irradiation conditions. On average, each domain is formed by grooves with a lateral period of 260-270 nm and a depth about 80 nm. By combination of scanning and transmission electron microscopy, magneto-optical imaging, and conductive atomic force microscopy techniques, we conclude that the boundaries of the LIPSS-covered domains play a prominent role in the magnetic flux diversion process within the film. This is confirmed by dedicated modelling of the flux dynamics, combined with the inversion of the magneto-optical signal. The created metasurfaces enable control of the flux penetration process at the microscale.

Evidence for the Presence of Borrelia burgdorferi Biofilm in Infected Mouse Heart Tissues.

Borrelia burgdorferi, the bacterium responsible for Lyme disease, has been shown to form antimicrobial-tolerant biofilms, which protect it from unfavorable conditions. Bacterial biofilms are known to significantly contribute to severe inflammation, such as carditis, a common manifestation of Lyme disease. However, the role of B. burgdorferi biofilms in the development of Lyme carditis has not been thoroughly investigated due to the absence of an appropriate model system. In this study, we examined heart tissues from mice infected with B. burgdorferi for the presence of biofilms and inflammatory markers using immunohistochemistry (IHC), combined fluorescence in situ hybridization FISH/IHC, 3D microscopy, and atomic force microscopy techniques. Our results reveal that B. burgdorferi spirochetes form aggregates with a known biofilm marker (alginate) in mouse heart tissues. Furthermore, these biofilms induce inflammation, as indicated by elevated levels of murine C-reactive protein near the biofilms. This research provides evidence that B. burgdorferi can form biofilms in mouse heart tissue and trigger inflammatory processes, suggesting that the mouse model is a valuable tool for future studies on B. burgdorferi biofilms.

Development of Novel Surface-Enhanced Raman Spectroscopy-Based Biosensors by Controlling the Roughness of Gold/Alumina Platforms for Highly Sensitive Detection of Pyocyanin Secreted from Pseudomonas aeruginosa.

Pyocyanin is considered a maker of Pseudomonas aeruginosa (P. aeruginosa) infection. Pyocyanin is among the toxins released by the P. aeruginosa bacteria. Therefore, the development of a direct detection of PYO is crucial due to its importance. Among the different optical techniques, the Raman technique showed unique advantages because of its fingerprint data, no sample preparation, and high sensitivity besides its ease of use. Noble metal nanostructures were used to improve the Raman response based on the surface-enhanced Raman scattering (SERS) technique. Anodic metal oxide attracts much interest due to its unique morphology and applications. The porous metal structure provides a large surface area that could be used as a hard template for periodic nanostructure array fabrication. Porous shapes and sizes could be controlled by controlling the anodization parameters, including the anodization voltage, current, temperature, and time, besides the metal purity and the electrolyte type/concentration. The anodization of aluminum foil results in anodic aluminum oxide (AAO) formation with different roughness. Here, we will use the roughness as hotspot centers to enhance the Raman signals. Firstly, a thin film of gold was deposited to develop gold/alumina (Au/AAO) platforms and then applied as SERS-active surfaces. The morphology and roughness of the developed substrates were investigated using scanning electron microscopy (SEM) and atomic force microscopy (AFM) techniques. The Au/AAO substrates were used for monitoring pyocyanin secreted from Pseudomonas aeruginosa microorganisms based on the SERS technique. The results showed that the roughness degree affects the enhancement efficiency of this sensor. The high enhancement was obtained in the case of depositing a 30 nm layer of gold onto the second anodized substrates. The developed sensor showed high sensitivity toward pyocyanin with a limit of detection of 96 nM with a linear response over a dynamic range from 1 µM to 9 µM.

Influence of lead concentration on Debye temperature in palladium alloys and microstructure

This article is about palladium-based membrane alloys with promising characteristics. Lead concentration in samples is 5 and 20 wt%. The samples are prepared from high purity metals (99.95 wt%). The samples are characterized using X-ray diffraction (XRD), scanning electron microscopy (SEM) and atomic force microscopy (AFM) techniques. Effect of the concentration of alloying components on the Debye temperature and on the mean-square displacements of atoms is determined. Influence of defects of the first class (point defect – vacancy pairs, pores, dislocation loops of small radius) found to be dominant in alloys.

Impact of fractal dimension and lateral correlation length on surface plasmon resonance activity in sputtered silver layers

Fractal and optical characteristics of self-affine surfaces of silver(Ag) thin films deposited through direct current (dc) magnetron sputtering as a function of thickness are investigated and explored here. The surface morphology of Ag thin films is characterized by field emission electron microscopy, and atomic force microscopy technique. The cube counting algorithm is used to extract the fractal dimension of Ag thin film. The surface roughness (interface width) shows monotonic increases with film thickness, while the other parameters, such as lateral correlation length, roughness exponent, and fractal dimension exhibit linear variation with thickness. Our findings reveal distinctive scaling behaviors, with scaling exponents α, β, and 1/z indicating unique growth characteristics. The interface width w increases as a power law of thickness t, w(t)∝tβ, with β=0.39± 0.007, and the lateral correlation length ξ grows as ξt∝t1/z with 1/z=0.14± 0.002. The roughness exponent extracted from height-height correlation analysis is α=0.61–0.41. The self-affine nature of the Ag thin films is further confirmed by the autocorrelation function. X-ray photoelectron spectroscopy (XPS) is used to the confirm the growth of Ag thin film. Additionally, we have studied the role of fractal dimensions and lateral correlation length (ξ) on the surface plasmon resonance (SPR) of Ag thin film. Our results indicate a red-shifting behavior of SPR with increasing interface width (w), lateral correlation length (ξ), and fractal dimensions. This study suggests the significance of not only the roughness exponent and fractal dimension but also the local surface slope in SPR activity in Ag thin films.

Benefits and Limitations of Encapsulating Platinum Electrocatalysts with Niobium Oxide

The development of energy infrastructure based on renewable sources is vital to reduce our reliance on fossil fuels. Technologies such as hydrogen fuel cells and water electrolyzers are able to bridge the gap between the intermittency issues associated with green energy sources such as wind and solar, and the demand for reliable electricity by being able to convert between electrical and chemical energy. Nanostructured and mesoporous platinum (Pt) prepared by electrodeposition or sputter coating have been shown to have increased performance in hydrogen fuel cells compared to the industry standard of Pt nanoparticles supported on carbon.1,2 Over the lifetime of a fuel cell Pt nanostructures and nanoparticles are, however, known to restructure and lose their surface area by mechanisms such as Ostwald ripening, dissolution, and coalescence. Previously, thin film Pt catalysts have been shown to be stabilized by a nanoscale film of niobium oxide.3 Herein, nanoscale thin films of niobium oxide are investigated as a stabilizing material through use by encapsulating nanostructured Pt catalysts.Nanostructured Pt catalysts were electrodeposited onto Pt-coated Si wafer substrates. Subsequently, niobium oxide films with thicknesses of 0.5 nm, 3 nm, and 4.5 nm were deposited onto the Pt catalyst using atomic layer deposition. X-ray fluorescence and conductive atomic force microscopy techniques were used to confirm the presence and coverage of the niobium oxide layer on the Pt catalyst. The performance of the encapsulated and un-encapsulated Pt catalysts as oxygen reduction reaction catalysts over the course of up to a thousand degradation cycles were evaluated using electrochemical techniques. The morphology of the catalyst before and after the degradation testing was also assessed using scanning electron microscopy techniques. Electrochemical impedance spectroscopy indicated that increasing the thickness of the niobium oxide layer increased the resistance of the catalyst towards the oxygen reduction reaction. The combined results of the analyses performed by electrochemical techniques and electron microscopy measurements revealed a range of film thicknesses for the niobium oxide that successfully stabilized the electrochemically active surface area and surface morphology of the Pt catalyst. Paul, M. T. Y.; Gates, B. D. Mesoporous Platinum Prepared by Electrodeposition for Ultralow Loading Proton Exchange Membrane Fuel Cells. Sci Rep 2019, 9, 4161.Debe, M. K. Tutorial on the Fundamental Characteristics and Practical Properties of Nanostructured Thin Film (NSTF) Catalysts. Electrochem. Soc. 2013, 160, F522.Eastcott, J.; Gates, B. D. Nanoscale Thin Films of Niobium Oxide on Platinum Surfaces: Creating a Platform for Optimizing Material Composition and Electrochemical Stability. Can. J. Chem. 2017, 96, 260–266.

Differentiation of Human Adipose-derived Stem Cells to Exosome-affected Neural-like Cells Extracted from Human Cerebrospinal Fluid Using Bioprinting Process.

Advancement in tissue engineering has provided novel solutions for creating scaffolds as well as applying induction factors in the differentiation of stem cells. The present research aimed to investigate the differentiation of human adipose-derived mesenchymal stem cells to neural-like cells using the novel bioprinting method, as well as the effect of cerebrospinal fluid exosomes. In the present study, the extent of neuronal proliferation and differentiation of adipose- derived stem cells were explored using the MTT method, immunocytochemistry, and real-- time PCR in the scaffolds created by the bioprinting process. Furthermore, in order to investigate the veracity of the identity of the CSF (Cerebrospinal fluid) derived exosomes, after the isolation of exosomes, dynamic light scattering (DLS), scanning electron microscopy (SEM), and atomic force microscopy (AFM) techniques were used. MTT findings indicated survivability and proliferation of cells in the scaffolds created by the bioprinting process during a 14-day period. The results obtained from real-time PCR showed that the level of MAP2 gene (Microtubule Associated Protein 2) expression increased on days 7 and 14, while the expression of the Nestin gene (intermediate filament protein) significantly decreased compared to the control. The investigation to confirm the identity of exosomes indicated that the CSF-derived exosomes had a spherical shape with a 40-100 nm size. CSF-derived exosomes can contribute to the neuronal differentiation of adipose- derived stem cells in alginate hydrogel scaffolds created by the bioprinting process.

Effect of morphology modulation and interface engineering of SnS-MoS2 heterojunction on nonlinear optical response

MoS2 base films with different morphologies were prepared by modulating the magnetron sputtering parameters, and the base films were used to induce the growth of SnS with different structures, forming columnar and worm-like SnS-MoS2 heterojunctions, which were found to have excellent nonlinear absorption properties and their properties could be modulated by the morphology of the films by Z-scanning tests. The tunable morphology and crystalline quality of the films were characterized using scanning electron microscopy, atomic force microscopy and X-ray diffraction techniques and explained using the Stranski-Krastanow growth mechanism. The Raman spectrum of the heterojunction shows the A1g vibrational peak at 320 cm−1 and the appearance of Sn4+ in the X-ray photoelectron spectroscopy confirms the existence of S-Sn-S charge transfer channels between the interfaces. The fine spectra of all the elements in the X-ray photoelectron spectroscopy data as well as the characteristic absorption peaks in the absorption spectra confirm the formation of heterojunctions, and the constructed heterojunctions are determined to be type-II heterojunctions using the method of the core energy level. Heterojunction was determined to be a type-II heterojunction by using the core energy level method. The photoluminescence peak quenching of the heterojunction indicates that there is a process of charge transfer between the interfaces, and the type-II heterostructure of SnS-MoS2 makes the nonlinear absorption performance in the 800 nm band regulated by the morphology of the material. The nonlinear optical absorption coefficient is two orders of magnitude higher than that of the pure materials, and the nonlinear absorption performance of the worm-like SnS-MoS2 heterojunction is superior to that of the columnar SnS-MoS2 heterojunction, which is attributed to the larger interfacial contact area, the better crystalline quality, and the more efficient carrier interfacial transport capability. These tunable type-II SnS-MoS2 heterojunctions with ultrafast nonlinear optical absorption have a positive impact on practical applications such as optical limiter devices and all-optical switching devices.

A Comparative Study of Methods for Calculating the Dislocation Density in GaN-on-Si Epitaxial Wafers.

A series of characterization methods involving high-resolution X-ray diffraction (HR-XRD), electron channel contrast imaging (ECCI), cathodoluminescence microscopy (CL), and atomic force microscopy (AFM) were applied to calculate the dislocation density of GaN-on-Si epitaxial wafers, and their performance was analyzed and evaluated. The ECCI technique, owing to its high lateral resolution, reveals dislocation distributions on material surfaces, which can visually characterize the dislocation density. While the CL technique is effective for low-density dislocations, it is difficult to accurately identify the number of dislocation clusters in CL images as the density increases. The AFM technique analyzes surface dislocation characteristics by detecting surface pits caused by dislocations, which are easily affected by sample and probe conditions. A prevalent method for assessing the crystal quality of GaN is the rocking curve of HR-XRD (ω-scan), which calculates the dislocation density based on the FWHM value of the curves. By comparing the above four dislocation characterization methods, the advantages and limitations of each method are clarified, which also verifies the applicability of DB=β29b2 for GaN-on-Si epitaxial wafers. This provides an important reference value for dislocation characterization in GaN-on-Si materials. The accuracy evaluation of dislocation density can truly and reliably reflect crystal quality, which is conducive to further optimization. Furthermore, this study can also be applied to other heterogeneous or homogeneous epitaxial materials.

Unraveling the mystery of sandwich structure: Emerging photocatalytic hydrogen production by g-C3N5 coupled Nb2C MXene forming Schottky heterojunction

The development of new photocatalysts and photocatalytic systems is the essence of the development of photocatalytic hydrogen production engineering. Nitrogen-rich graphite carbon nitride (g-C3N5) has gradually replaced conventional graphite phase carbon nitride (g-C3N4) with a smaller bandgap and high-efficiency visible light utilization. In this study, g-C3N5 and Nb2C MXene coupled composition with sandwich structure were manufactured by a simple ultrasonic magnetic stirring method and used for photocatalytic hydrogen production. By adjusting the ratios of single components in the system, the hydrogen production rate of the optimal sample 4:1g-C3N5/Nb2C under visible light irradiation is 2529.5 μmol·g−1·h−1, which is 21 times higher than that of g-C3N5. The high apparent quantum yield (AQY) value of 17.3 % also proves a high light utilization rate. The atomic force microscopy (AFM) technique reveals variations in the thickness of the samples, while strongly demonstrating the formation of sandwich structure. In addition, X-ray photoelectron spectroscopy (XPS) analysis further reveals the electron transfer paths within the system, preliminarily verifying the formation of Schottky heterojunctions. Kelvin probe force microscopy (KPFM) tests not only re-validate the correctness of the electron transfer path but also demonstrate the accuracy of the energy bands. The density-functional theory (DFT) calculations corroborate that Nb2C MXene plays the role of a photoco-catalyst to form Schottky heterojunctions with g-C3N5 for efficient carrier separation and migration. This work highlights the key role of sandwich structure photocatalytic systems on photocatalytic performance.

Grape Seed Extract as an Environment-Friendly Green Inhibitor for Corrosion of Mild Steel in 1 M Sulfamic Acid

AbstractA corrosion inhibition study of mild steel in 1 M sulfamic acid was conducted using grape seed extract (GSE) as a possible green inhibitor. Electrochemical techniques were adopted to measure the corrosion rate in both the absence and presence of the GSE. Conditions were standardized to obtain optimum inhibition efficiency by varying the concentration of inhibitor and temperature. The kinetic parameters were calculated using the Arrhenius equation. Surface analysis was conducted by scanning electron microscope (SEM) and atomic force microscope (AFM) techniques. A suitable mechanism was proposed for the corrosion inhibition process. Grape seed extract showed a maximum efficiency of 65%, with a concentration of 0.24 g/L at 303 K from potentiodynamic polarization (PDP) studies. With the increase in temperature, the efficiency decreased, resulting in the GSE inhibitor’s physical adsorption. Surface morphology studies supported the adsorption of GSE on mild steel. GSE acted as an efficient green inhibitor with environmental benefits.

Verbena officinalis (VO) leaf extract as an anti-corrosion inhibitor for carbon steel in acidic environment

In the present work, Verbena Officinalis (VO) leaf extract was used as potential corrosion inhibitor for the corrosion of carbon steel (CS) in 0.5 M H2SO4 medium. Further, the corrosion inhibiting nature of VO leaf extract towards the CS was evaluated using mass loss (ML), potentiodynamic polarization (PDP), electrical impedance spectroscopy (EIS) and surface morphological analyses using atomic force microscope (AFM) and X-ray photoelectron spectroscopy (XPS) techniques. Calculation of activation energy Ea∗\\documentclass[12pt]{minimal} \\usepackage{amsmath} \\usepackage{wasysym} \\usepackage{amsfonts} \\usepackage{amssymb} \\usepackage{amsbsy} \\usepackage{mathrsfs} \\usepackage{upgreek} \\setlength{\\oddsidemargin}{-69pt} \\begin{document}$$\\left( {{\ ext{E}}_{{\ ext{a}}}^{*} } \\right)$$\\end{document} using Arrhenius equation shows the increase in activation energy when adding the VO leaf extract in 0.5 M H2SO4 medium and the maximum activation energy (Ea∗\\documentclass[12pt]{minimal} \\usepackage{amsmath} \\usepackage{wasysym} \\usepackage{amsfonts} \\usepackage{amssymb} \\usepackage{amsbsy} \\usepackage{mathrsfs} \\usepackage{upgreek} \\setlength{\\oddsidemargin}{-69pt} \\begin{document}$${\ ext{E}}_{{\ ext{a}}}^{*}$$\\end{document} = 49.9 kJ mol−1) was observed for 1000 mg L−1 VO leaf extract in acid medium. The negative free energy values suggested the spontaneous and the stability of the adsorbed layer of VO leaf extract on the CS surface. Using EIS measurements, high percent inhibitory effectiveness of 91.1% for 1000 ppm solutions was achieved. With an increase in VO leaf extract dose, the double layer capacitance (Cdl) values fall while the values of charge transfer (Rct) increase. This showed that a protective layer of VO leaf extract on CS surface was formed. The polarization curves showed that the VO leaf extract acts as a mixed-type inhibitor. It is discovered that the adsorption of VO leaf extract molecules adhering to the CS surface followed the Langmuir isotherm. The anti-corrosion action of VO leaf extract is fully demonstrated by some surface techniques.

Preparation of pyridoxine-based polyurethane modified sensors and their use in simultaneous determination of Cu(II) – Co(II) ions

In this study, pyridoxine-based polyurethane-modified electrodes were prepared to simultaneously and sensitively measure copper (Cu(II)) and cobalt (Co(II)) ions in complex matrix samples. For the production of the electrodes, firstly, the synthesis of pyridoxine-based polyurethane structures was carried out. In these syntheses, the polymer structure was diversified by using different isocyanates. Polyethyleneglycol-200 (PEG), pyridoxine (B6), and β-cyclodextrin (β-CD) groups were used as the source of polyol. The synthesized polyurethane structures were characterized by different instrumental techniques and used in gold electrode surface modification. Modified sensor surfaces were examined by scanning electron microscopy and atomic force microscopy techniques. The prepared modified sensors were used for the simultaneous detection of Cu(II) and Co(II) ions using the differential pulse voltammetry technique. The limit of detection (LOD), limit of quantitation (LOQ), and R2 values for Cu(II) ions were calculated as 8.81 μM, 29.4 μM, and 0.993, respectively. LOD, LOQ, and R2 values for Co(II) ions were calculated as 9.84 μM, 32.8 μM, and 0.9935, respectively. For repeatability, the relative standard deviation (RSD %) of the prepared simultaneous sensors was determined as 1.54 and 1.71 for Cu(II) and Co(II), respectively. As a result, Cu(II) and Co(II) ions were measured independently and simultaneously with high sensitivity. According to these results, it is predicted that pyridoxine-based polyurethane-modified sensors may be suitable for the simultaneous detection of Cu(II) and Co(II) in medical, food, and agricultural samples.

From Nanoscale to Macroscale Characterization of Sulfur-Modified Oxidized Carbon Nanotubes in Styrene Butadiene Rubber Compounds.

The homogeneous dispersion of carbon nanotubes (CNTs) in a rubber matrix is a key factor limiting their amazing potential. CNTs tend to agglomerate into bundles due to van der Waals interactions. To overcome this limitation, CNTs have been surface-modified with oxygen-bearing groups and sulfur. Using atomic force microscopy (AFM) techniques, a deep nanoscale characterization of the morphology, the degree of dispersion of the CNTs in the styrene butadiene rubber (SBR) matrix, and the thickness of the interfacial layer was carried out in this study. In this context, the results from nanoscale characterization showed that the thermal oxidation-sulfur treatment leads to a composite with better dispersion in the matrix, as well as a thicker interfacial layer, indicating a stronger filler-rubber interaction. The second part of this work focused on the macroscale results, such as the Payne effect, vulcanization curves, and mechanical properties. The Payne effect, vulcanization curves, and mechanical properties confirmed the lower reinforcing effect observed in the case of the chemical oxidation treatment because, on the one hand, this composite showed the highest agglomeration of CNTs after the acid treatment. On the other hand, the presence of acid residues provoked the absorption of basic accelerators on the surface of the CNTs.