Methodology For Characterization Research Articles

Surface Enhancement of Titanium-Based Coatings on Commercial Hard Steel Cutting Tools

This study investigates the mechanical properties, surface integrity, and chemical configuration of PVD-coated high-speed steel (HSS) cutting tools, with a particular focus on titanium nitride (TiN) and titanium aluminium nitride (TiAlN) coatings. A range of characterisation methodologies were employed to examine the impact of pre-coating surface conditions on the resulting coatings. This impact includes the effects of gas bubble production and unequal distribution of elements, which are two unwanted occurrences. Notwithstanding these difficulties, coatings applied on surfaces that were highly polished exhibited more consistency in their mechanical and elemental characteristics, with a thickness ranging from 2 to 4 µm. The study of mechanical characteristics confirms a significant increase in hardness, from an initial value of roughly 1000 HV0.5 for untreated tools to 1300 HV0.5 for tools with physical vapour deposition (PVD) coatings. Although PVD coatings produced on an industrial scale might not exceed the quality of coatings manufactured in a laboratory, they do offer substantial enhancements in terms of hardness. This study highlights the significant importance of thorough surface preparation in achieving enhanced coating performance, hence contributing to the efforts to prolong the lifespan of tools and enhance their performance even under demanding operational circumstances.

An Enhanced Approach for High-Strain Plasticity in Flat Anisotropic Specimens with Progressively Distorting Neck Sections

An Enhanced Approach for High-Strain Plasticity in Flat Anisotropic Specimens with Progressively Distorting Neck Sections

A methodology for phase characterization in pellet feed using digital microscopy and deep learning

This work proposes a new method for characterizing pellet feed, employing Deep Learning (DL) and Convolutional Neural Networks (CNNs). The main minerals in the composition of the studied pellet feed are hematite, magnetite, goethite, and quartz. Over time, several characterization methodologies have been developed that use Digital Microscopy and Image Analysis tools. The greatest difficulties in this characterization lie in differentiating the textures of hematite particles, the different shapes of their crystals, or discriminating between quartz and resin in reflected light optical microscopy images. This work proposes a mineral characterization methodology based on the Mask R-CNN algorithm. The goal is to perform instance segmentation, that is, to identify, classify, and segment objects in the images. Two DL models were combined: the BF Model performs instance segmentation for the compact, porous, martite, and goethite classes in images obtained in Bright Field mode, and the CPOL Model uses images acquired in Circularly Polarized Light to segment the monocrystalline, polycrystalline, and martite classes. An F1-score of around 80% was obtained for the BF Model and around 90% for the CPOL Model. The results were promising and can be improved as the training image database increases.

Integrated Approach of Historical Landscape Characterisation Techniques and Remote Sensing for the Definition of Predictive Models and Scenario Analysis in the Planning of Archaeological Areas

This study explores the synergistic integration of remote sensing (RS) and Historical Landscape Characterisation (HLC) methodology as an innovative, multi-scalar and holistic approach to enhance archaeological planning. The goal is to maximize the effectiveness of the investigations, optimizing data collection and improving the contextual understanding of the sites. In fact, these methodologies can significantly contribute to the documentation, conservation, planning and valorisation of archaeological areas. By integrating RS data with features detected by HLC, a complete picture is obtained that facilitates a deeper understanding of the landscape and historical dynamics. This article will explain the combined approach of RS and HLC, presenting some methodologies key to improving the precision and effectiveness of archaeological planning. This integration facilitates the sustainable preservation of archaeological resources and contributes to the conscious management of cultural heritage in the context of contemporary development. The paper demonstrates, through a case study, how the application of the two methodologies (RS and HLC) in an integrated form can provide an exhaustive interpretation of the territory in which the archaeological area is located, which can represent an exhaustive knowledge base on which to set up effective processes for the strategic territorial planning of archaeological areas.

Functionalized Binders Boost High‐Capacity Anode Materials

AbstractThe burgeoning field of energy storage battery innovation has sparked a relentless pursuit of high‐capacity anode materials to meet the escalating demand for improved energy density. Typically, these materials for batteries experience significant volume changes during cycles, which severely test the structural integrity and lifespan of electrode configurations. High‐performance binders have emerged as a critical component in addressing this challenge. Although they represent a small proportion of the battery's composition, binders play a pivotal role in enhancing electrochemical efficiency, safety, and cost‐effectiveness of batteries. The advancement of high‐capacity anode materials has rendered traditional binders inadequate, prompting the development of functional binders that are increasingly being refined to meet these requirements. This article began by outlining the role and requirements of binders within electrodes, examining cutting‐edge characterization methodologies, and discussing the “structure‐function” paradigm that underpins binder selection. It then showcased the research advancements in identifying suitable binders for high‐capacity anode materials, including silicon (Si), phosphorus (P), tin (Sn), antimony (Sb), and germanium (Ge). In summary, the article contemplated the future direction of binder development and application in high‐capacity electrode materials. The aim is to facilitate the progression of high‐performance, high‐capacity anodes, thereby accelerating the development of high‐energy‐density lithium‐ion and sodium‐ion batteries.

Characterization of Freezing Processes in Drug Substance Bottles by Ice Core Sampling

Freezing of biological drug substance (DS) is a critical unit operation that may impact product quality, potentially leading to protein aggregation and sub-visible particle formation. Cryo-concentration has been identified as a critical parameter to impact protein stability during freezing and should therefore be minimized. The macroscopic cryo-concentration, in the following only referred to as cryo-concentration, is majorly influenced by the freezing rate, which is in turn impacted by product independent process parameters such as the DS container, its size and fill level, and the freezing equipment. (At-scale) process characterization studies are crucial to understand and optimize freezing processes. However, evaluating cryo-concentration requires sampling of the frozen bulk, which is typically performed by cutting the ice block into pieces for subsequent analysis. Also, the large amount of product requirement for these studies is a major limitation. In this study, we report the development of a simple methodology for experimental characterization of frozen DS in bottles at relevant scale using a surrogate solution. The novel ice core sampling technique identifies the axial ice core in the center to be indicative for cryo-concentration, which was measured by osmolality, and concentrations of histidine and polysorbate 80 (PS80), whereas osmolality revealed to be a sensitive read-out. Finally, we exemplify the suitability of the method to study cryo-concentration in DS bottles by comparing cryo-concentrations from different freezing protocols (-80°C vs -40°C). Prolonged stress times during freezing correlated to a higher extent of cryo-concentration quantified by osmolality in the axial center of a 2 L DS bottle.Graphical

Extraction of bioactive compounds from Vitex megapotamica: A study and selection of variables

AbstractFruits are widely used to obtain and study bioactive compounds. Among them, the tarumã (Vitex megapotamica) is still understudied. The extraction of bioactive compounds from the powdered pulp of the ripe fruit of the tarumã was studied from the selection of several variables of the extraction process through the experimental design Plackett–Burman: the pH, the solid:liquid ratio, agitation, and temperature in an extraction time of 3 h. The extracts obtained were evaluated for antioxidant activity by 2,2′‐azino‐bis‐(3‐ethylbenzothiazoline‐6‐sulfonic acid) (ABTS), 2,2‐diphenyl‐1‐picrylhydrazyl (DPPH), and for total phenolic compounds, as well as the presence of flavonoids, anthocyanins, carotenoids, and identification of bioactive compounds was assessed by high‐performance liquid chromatography (HPLC). Using the experimental design, the best extraction condition was defined with a pH of 5, solid:liquid ratio of 1:30, stirring at 100 rpm, with a temperature of 80°C, obtaining 104.21 mg Gallic Acid Equivalent (GAE) 100 g−1 for phenolic compounds total, 742.71 μmol Trolox g−1 for ABTS, and EC50 of 2884.98 mg L−1 for DPPH. From HPLC, the presence of fumaric acid, gallic acid, p‐coumaric acid, and caffeic acid in the extracts was detected. Regarding flavonoids, anthocyanins, and carotenoids, the values obtained were 6.38 mg ECG g−1, 1.67 mg ECG g−1, and 2.89 mg 100 g−1, respectively. The selection of extraction conditions allowed obtaining better levels of bioactive compounds in the powdered pulp of tarumã extract, even with the use of water as a solvent, to avoid the presence of chemical residues in the extract, with antioxidant potential and viability for application in food products.Practical applicationsRecent research suggests a change in perspective regarding the consumption of healthier foods from plants and fruits that have important health properties. In this regard, tarumã (Vitex megapotamica) fruit has been standing out as a potential source of bioactive compounds with significant medicinal properties. The extracts obtained have a significant amount of phenolic compounds, as well as the presence of flavonoids, anthocyanins, and carotenoids, in which all of these have great potential bioactive activities. Thus, a good methodology of extraction and characterization of tarumã extract becomes a crucial part of any food, chemical, or pharmaceutical industry sector. In this regard, the present study with experimental design Plackett–Burman extraction is the way ahead due to high bioactive retention and the cost implications of the process.

Colouring solutions for building integrated photovoltaic modules: A review

As global decarbonisation requires the widespread adoption of solar photovoltaic (PV) electricity, addressing challenges related to land use has become relevant. The conflict between PV installations and other land uses, such as forestry or agriculture, highlights the urgency for alternative solutions. Integrating PV technology into the built environment is a compelling strategy to mitigate these challenges, enabling electricity generation precisely where it is needed. In the context of buildings integrated photovoltaics (BIPV), PV modules serve a dual purpose, functioning both as electricity generators and integral components of the architectural design. Therefore, the architecture requirements — specifically in terms of shape, size, and colour— become relevant for BIPV modules. This paper offers a general overview of the diverse colouring technologies employed for BIPV modules, describing their functioning, challenges, and advantages. An examination of the current landscape of coloured PV products involving considerations of pricing and power output is presented. Additionally, this work addresses the critical topics of reliability and stability in colour solutions, outlining methodologies for quantitative colour characterization. It provides foresight into the potential challenges facing installations in the future and explores the multifaceted social, economic, and environmental implications of this evolving technology.

Rational Design of Amorphous Nanomaterials for Enhanced Electrochemical CO2 and Nitrate Reduction

Amorphous materials are distinguished by their exceptional attributes, notably their expansive surface area and the profusion of active sites they present. Consequently, the amorphization process stands as an efficacious strategy to augment the catalytic efficacy of electrocatalysts. This is achieved through the meticulous construction of the surface architecture and the precise modulation of the electronic configuration of these materials. Therefore, this review aims to offer a thorough examination of the latest progress in the application of amorphous materials for the enhancement of electrocatalytic processes, with a particular emphasis on the nitrate (NO3‐) reduction reaction (NITRR) and the carbon dioxide reduction reaction (CO2RR). Initially, we delve into the structural benefits inherent to amorphous materials, outlining the diverse synthesis techniques and characterization methodologies utilized in their development. Following this, we illustrate the utilization of various amorphous materials in NITRR and CO2RR, accentuating how the amorphous framework influences electrocatalytic activities. Concludingly, we encapsulate the merits and the obstacles encountered in the application of amorphous electrocatalysts for NITRR and CO2RR, whilst also forecasting the future direction for the creation of innovative amorphous electrocatalysts.

Effect of Quorum Sensing Molecules on the Quality of Bacterial Nanocellulose Materials.

Bacterial nanocellulose (BNC) biofilms, produced by various bacterial species, such as Gluconacetobacter xylinus, represent a highly promising multifunctional material characterized by distinctive physiochemical properties. These biofilms have demonstrated remarkable versatility as nano biomaterials, finding extensive applications across medical, defense, electronics, optics, and food industries. In contrast to plant cellulose, BNC biofilms exhibit numerous advantages, including elevated purity and crystallinity, expansive surface area, robustness, and excellent biocompatibility, making them exceptional multifunctional materials. However, their production with consistent morphological properties and their transformation into practical forms present challenges. This difficulty often arises from the heterogeneity in cell density, which is influenced by the presence of N-acyl-homoserine lactones (AHLs) serving as quorum sensing signaling molecules during the biosynthesis of BNC biofilms. In this study, we employed surface characterization methodologies including scanning electron microscopy, energy-dispersive spectroscopy, diffuse reflectance infrared Fourier transform spectroscopy, and atomic force microscopy to characterize BNC biofilms derived from growth media supplemented with varying concentrations of distinct N-acyl-homoserine lactone signaling molecules. The data obtained through these analytical techniques elucidated that the morphological properties of the BNC biofilms were influenced by the specific AHLs, signaling molecules, introduced into the growth media. These findings lay the groundwork for future exploration of leveraging synthetic biology and biomimetic methods for tailoring BNC with predetermined morphological properties.

Challenges and Advances in Wide‐Temperature Electrolytes for Lithium‐Ion Batteries

AbstractLithium‐ion batteries (LIBs) have gained widespread attention due to their numerous advantages, including high energy density, prolonged cycle life, and environmental friendliness. Nevertheless, their electrochemical performance deteriorates rapidly under extreme temperature conditions, accompanied by a series of safety issues. Electrolyte optimization has emerged as a crucial and feasible strategy to expand the operational temperature range of LIBs. This review comprehensively summarizes the challenges, advances, and characterization methodologies of electrolytes at both subzero and elevated temperatures. Initially, it discusses the degradation mechanisms of different types of electrolytes at extreme temperatures, integrates recent advances, and offers insights into future research directions. Subsequently, various experimental techniques are systematically presented to evaluate the fundamental physical properties, stability, and dynamic behaviors of electrolytes in non‐ambient environments. Finally, it also provides relevant computational methods across the electronic, molecular, and macroscopic scales, and explores the application of high‐throughput techniques in this field. This review offers valuable guidance for breaking the working temperature limits of electrolytes and promoting the development of next‐generation LIBs.

Expression of Concern: Agricultural waste biomass for sustainable bioenergy production: Feedstock, characterization and pre-treatment methodologies

Expression of Concern: Agricultural waste biomass for sustainable bioenergy production: Feedstock, characterization and pre-treatment methodologies

Dissolution Heterogeneity Observed in Anisotropic Ruthenium Dioxide Nanocrystals via Liquid-Phase Transmission Electron Microscopy.

Noble metal oxides such as ruthenium dioxide are highly active electrocatalysts for anodic reactions in acidic electrolytes, but dissolution during electrochemical operation impedes wide-scale applications in renewable energy technologies. Improving the fundamental understanding of the dissolution dynamics of application-relevant morphologies such as nanocrystals is critical for the grid-scale implementation of these materials. Herein, we report the nanoscale heterogeneity observed via liquid-phase transmission electron microscopy during ruthenium dioxide nanocrystal dissolution under oxidizing conditions. Single-crystalline ruthenium dioxide nanocrystals enabled the direct observation of dissolution along different crystallographic facets, allowing an unprecedented direct comparison of crystal facet stability. The nanoscale observations revealed substantial heterogeneity in the relative stability of crystallographic facets across different nanocrystals, attributed to the nanoscale strains present in these crystals. These findings highlight the importance of nanoscale heterogeneity in determining macroscale properties such as electrocatalyst stability and provide a characterization methodology that can be integrated into next-generation electrocatalyst discovery efforts.

New approach methodologies to enhance human health risk assessment of immunotoxic properties of chemicals - a PARC (Partnership for the Assessment of Risk from Chemicals) project.

As a complex system governing and interconnecting numerous functions within the human body, the immune system is unsurprisingly susceptible to the impact of toxic chemicals. Toxicants can influence the immune system through a multitude of mechanisms, resulting in immunosuppression, hypersensitivity, increased risk of autoimmune diseases and cancer development. At present, the regulatory assessment of the immunotoxicity of chemicals relies heavily on rodent models and a limited number of Organisation for Economic Co-operation and Development (OECD) test guidelines, which only capture a fraction of potential toxic properties. Due to this limitation, various authorities, including the World Health Organization and the European Food Safety Authority have highlighted the need for the development of novel approaches without the use of animals for immunotoxicity testing of chemicals. In this paper, we present a concise overview of ongoing efforts dedicated to developing and standardizing methodologies for a comprehensive characterization of the immunotoxic effects of chemicals, which are performed under the EU-funded Partnership for the Assessment of Risk from Chemicals (PARC).

Ferroelectric Polarization‐Mediated Modulation of Optical Properties in 2D van der Waals Architectures

AbstractThe integration of 2D ferroelectric materials with 2D photoelectric materials presents a promising avenue for addressing issues related to controlled doping and device integration in layered semiconductors. The reversible and non‐volatile residual polarization inherent to ferroelectrics can provide stable n‐ or p‐type doping for 2D semiconductors. Despite advances in doping strategies for 2D materials, existing techniques, and post‐doping characterization methodologies exhibit limitations, including the challenge of achieving high‐resolution graphical depictions of doped structures. Here, a WS2/CuInP2S6 heterostructure is demonstarted whereby the residual polarization of ferroelectric CuInP2S6 regions with anti‐parallel directions supplies screening charges of opposite signs to WS2 monolayers. This notably alters the ratio of neutral excitons and negatively charged trions within the recombination luminescence of the direct‐gap semiconductor, thereby offering a viable approach for controllable, non‐volatile modulation in 2D systems. Beyond proposing a feasible strategy for patterned doping and effective regulation in 2D semiconductors through interface engineering, this work enhances the understanding of the interplay between ferroelectrics and semiconductors.

Using Capillary Electrophoresis to Investigate Protein Conformational and Compositional Heterogeneity.

Detailed insights into protein structure/function relationships require robust characterization methodologies. Free-solution capillary electrophoresis (CE) is a unique separation technique which is sensitive to the conformation and/or composition of proteins, and therefore provides information on the heterogeneity of these properties. Three unrelated, conformationally/compositionally-altered proteins were separated by CE. An electrophoretic mobility distribution was determined for each protein along with its conformational and/or compositional heterogeneity. CE results were compared with molar mass distributions obtained from size-exclusion chromatography coupled to light scattering (SEC-MALS). Bovine serum albumin oligomers and two monomeric species were separated, highlighting variations in conformational/compositional heterogeneity among the oligomers. Analysis of yeast alcohol dehydrogenase resolved two monomeric conformers and various tetrameric species, illustrating the impact of zinc ion removal and disulfide bond reduction on the protein's heterogeneity. The apo (calcium-free) and holo forms of bovine α-lactalbumin were separated and differences in the species' heterogeneity was measured; by contrast, the SEC-MALS profiles were identical. Comparative analysis of these structurally unrelated proteins provided novel insights into the interplay between molar mass and conformational/compositional heterogeneity. Overall, this study expands the utility of CE by demonstrating its capacity to discern protein species and their heterogeneity, properties which are not readily accessible by other analytical techniques.

Hybrid search methodology for mechanical characterization of material produced via WAAM assuming Gurson porous material

Hybrid search methodology for mechanical characterization of material produced via WAAM assuming Gurson porous material

Monitoring the Degradation of Metal‐Organic Framework Drug Nanocarriers by In‐situ NMR Spectroscopy

An accurate characterization methodology is indispensable to design nanoparticle‐based drug delivery system (DDS) adapted to specific diseases and therapies. However, characterization techniques employed to investigate drug release and nanoparticle degradation require separating the nanoparticles from their suspension media, which can lead to artefacts. Therefore, there is a clear need to implement novel versatile in‐situ methods. Here, we report the use of in‐situ NMR spectroscopy to monitor drug delivery processes from MOF nanocarriers, both in solution and in the solid state simultaneously. In‐situ1H NMR investigation of nanoMIL‐100(Al) suspension in phosphate medium enabled recording the trimesate ligand loss in the solid phase and the ligand release in the liquid phase as a function of time. Simultaneously, 27Al NMR enabled assessing the progressive replacement of carboxylate ligands by phosphates leading to the formation of new aluminum species. Using the same strategy, we also compared the degradation of nanoMIL‐100(Al) loaded with two drug analogs, highlighting an effect of metal‐ligand complexing strength. Furthermore, our in‐situ technique is applicable to studying the reaction of paramagnetic nanoMIL‐100(Fe) in the liquid phase. This work offers an alternative to ex‐situ techniques for understanding the degradation mechanism of MOF nanocarriers and could be an asset for other nanoscale DDSs.

STUDIES TO ESTABLISH THE SCALING FACTOR METHODOLOGY FOR LIQUID RADIOACTIVE WASTE GENERATED BY TRIGA REACTOR

During TRIGA reactor operation significant amounts of liquid radioactive waste are generated requiring appropriate management to ensure their safe disposal. Radiological characterization is an important activity needed to accomplish the waste acceptance criteria for different management steps including disposal. The purpose of this paper is to assess the activity concentrations of the (_1^3)H , (_38^90)Sr, (_28^63)Ni (difficult-to-measure), and gamma emitters (easy-to-measure) radionuclides in liquid radioactive waste generated by the TRIGA reactor operation and to establish a correlation among them to determine the scaling factors for this waste category. The radiological protocols applied for (_28^63)Ni and (_38^90)Sr, separation and purification involve extraction chromatography using selective resins, while for (_1^3)H separation the distillation technique was applied. The assessment of gamma emitters was carried out using gamma-ray spectrometry and the detection of (_1^3)H , (_38^90)Sr, and (_28^63)Ni was performed by liquid scintillation counting. The chemical yield of each experiment was determined by measuring the carrier added in each test by inductively coupled plasma optical emission spectrometry. The activity concentrations of (_38^90)Sr, and (_28^63)Ni obtained were correlated with the activity concentration of (_27^60)Co for establishing the scaling factor for the liquid radioactive waste stream. There were obtained good correlations but more experimental data are needed to determine the relevant scaling factors for these difficult-to-measure radionuclides. The scaling factors, once established, will improve and optimize the radiological characterization methodology applied for liquid radioactive waste as an easy and rapid method for assessment of concentration activities of difficult-to-measure radionuclides. Until now, no scaling factors data were reported for this liquid radioactive waste generated by TRIGA reactor operated by Institute for Nuclear Research Pitesti. The results obtained in this work represent preliminary data for establishing correlations between difficult-to-measure and easy-to-measure radionuclides and will be used for developing a scaling factor methodology. This will further be used to determine the inventory of difficult-to-measure radionuclides in different waste streams generated by TRIGA operation and decommissioning (foreseen after 2035).

Skin Penetrating Lipid Vesicles: Ethosomes in Drug Delivery and Cosmeceuticals

Ethosomes, or skin penetrating lipid vesicles, are proving to be effective delivery systems for cosmetics and pharmaceuticals. This article thoroughly examines ethosomes, including their structure, formulation methods, characterization tactics, and skin penetration mechanisms. Ethosomes are able to deform and penetrate the stratum corneum thanks to their special lipid compositions and elasticity, which let them get around obstacles in transdermal drug administration and cosmeceutical application. The selection of lipids, surfactants, and active compounds for ethosome formulations, as well as the function of ethanol as a penetration enhancer, are covered in detail in the current article. The discussion of various production processes and characterization methodologies emphasizes the significance of size distribution, zeta potential, and encapsulation effectiveness. The review investigates the mechanisms through which ethosomes interact with the stratum corneum and other skin barriers and the variables affecting the effectiveness and depth of their transdermal administration. The applications of ethosomes in the delivery of both hydrophilic and lipophilic medicines and their promise in targeted and localized treatments highlight their adaptability. The clinical implications are discussed, illuminating preclinical and clinical research that highlight the improved efficacy and safety of formulations based on ethosomes. Ethosomes provide a platform for improving the distribution of active substances like vitamins, antioxidants, and peptides in the field of cosmeceuticals. Their uses encompass topical formulations for skin whitening, hydration, rejuvenation, and antiaging and skin care products. The paper also discusses future directions in ethosome research, such as customized medicine and combination medicines, as well as regulatory issues and difficulties with commercialization.