Electron Microscopy-energy Dispersive X-ray Research Articles

Electrochemical Analysis Comparison of Nitrogen Undoped and Doped Ti3C2Tx/Co3O4 Hybrid Composites on Carbon Cloth for Application as Electrode in Supercapacitor

Supercapacitor provides great potential for good energy storage devices application, compared with other energy storage such as rechargeable batteries, fuel cell, dielectric capacitors and so on. Freestanding and flexible electrodes are vital for the development of flexible and wearable devices that store energy. But the significant trade-off between mechanical flexibility and electrode electrochemical performance limits the fabrication of efficient energy storage systems. In this research, we report the synthesis of a 2D material Ti3C2Tx and Co NPs on carbon cloth (CC) substrate. Co NPs was synthesized by microplasma reactors which eliminate harmful reducing agents and are efficient and cost-effective. And the Co NPs/Ti3C2Tx were synthesized by hydrothermal method for supercapacitor. These materials were characterized by scanning electron microscopy (SEM) Energy Dispersive Spectroscopy and X-Ray Diffraction for morphology and phases analysis. Besides these Transmission electron microscopies (TEM) and X-ray Photoelectron spectroscopy (XPS) were also done. For electrochemical analysis these materials were applied on the 2.25 cm2 carbon cloth as active material (working electrode) by various electrochemical techniques in 1 M H2SO4 electrolyte. The Co NPs/Ti3C2Tx electrode had a maximum gravimetric capacity of 52 mAh g-1, specific capacitance of 580 mF cm-2 and 240 F g-1 at the current density of 1 mA cm-2. Figure 1

Characterization and ohmic contact properties of indium tin-oxide films prepared on p-type GaN using electron-cyclotron-resonance plasma-sputter deposition

The optical and electrical properties of indium tin oxide (ITO) films deposited using electron cyclotron resonance (ECR) plasma-sputter deposition and the ohmic contact properties between the ITO films and p-type gallium nitride (p-GaN) were evaluated. The electrical properties of the ITO films were evaluated in terms of the dependence on the tin (IV) oxide (SnO2) content of the ITO target and radio frequency (RF) power. The ohmic contact properties between the ITO films and p-GaN were also characterized by varying the top-surface Mg concentration of the p-GaN substrate. An ohmic contact was achieved without post-annealing treatment by depositing the film on a p-GaN high-dope substrate with a top-surface Mg concentration of 2.0 × 1020 cm−3 under low RF-power deposition using an ITO sputter target with 10 wt.% SnO2. The interface between the ITO films and p-GaN that achieved an ohmic contact was observed using scanning transmission electron microscopy (STEM) and was very smooth with no crystal disorder. This indicates that the crystallinity of the ITO films and p-GaN surface is a factor affecting ohmic-contact properties. The inter-diffusion between the ITO films and p-GaN surface was also evaluated using transmission electron microscopy energy dispersive X-ray spectroscopy (TEM-EDS), and no inter-diffusion was observed.

Evaluation of the performance of air micro-nano bubbles for cleaning in place to reduce the reverse osmosis membrane clogging

This paper investigates the effect of air micro-nano bubbles (AMNBs) on increasing the efficiency of the cleaning in place (CIP) process for reverse osmosis (RO) systems used in petrochemical industries. A membrane from the desalination unit was extracted as the test section over which surface have been formed various types of clogging. The test set-up included, a Lab-Scale Plate-and-Frame Module (LSPFD) accompanied by a micro-nano bubble generator. The ratio of permeate flux and salt rejection in four states before CIP, after conventional CIP, after treatment with AMNBs, and after the conventional CIP along with AMNBs were recorded as 24.4, 26.9, 25.1, 27.3 and 68.2, 77.4, 70.1, 81.8 %, respectively. Scanning Electron Microscopy (SEM) images and Energy Dispersive X-ray Spectrometer (EDS) analysis clearly show a notable reduction in clogging on the membrane when AMNBs are employed. Therefore, cleaning intervals of the industrial RO membranes increase resulting in the extension of their life-span.

Temperature-induced variations in the structural, morphological and optical features of cobalt oxide nanoparticles synthesized via hydrothermal method

Cobalt oxide is a promising material that attracts the researchers to find its application in various fields like catalysts, dielectric applications, gas sensors and electronics devices, etc. In this work, we investigated the effect of temperature in the structural, elemental, morphological and optical properties of Co3O4 nanoparticles synthesized by hydrothermal method. The as-prepared and annealed samples were observed for their structural and optical properties. The structural analysis and micro-strain effects of Co3O4 nanoparticles with cubic spinel structure were carried out through X-ray diffraction (XRD) studies. The crystallite size of as-prepared and annealed samples were around 27 nm and 29 nm, respectively. Raman spectrum showed the lattice vibrations of both oxidation states of cobalt oxide nanoparticles. Elemental analysis were observed through X-ray photoelectron spectroscopy (XPS). The morphology and chemical composition of the samples were determined from the field emission scanning electron microscope (FESEM) image and energy dispersive X-ray spectroscopy (EDAX). Moreover, the internal structure of both samples were compared through transmission electron microscopic (TEM) studies. The optical studies were done using the absorption spectrum and photoluminescence spectroscopy. Two direct band gaps (1.8 and 3.2 eV) were observed in the as-prepared, which got red-shifted on annealing (1.7 and 2.5 eV) due to size effects. The charge transfer process in two oxidation states of cobalt oxide could be identified from these bandgaps. Emission peaks in the photoluminescence spectrum of samples are due to the recombination of free-excitons and point defects in the crystal lattice.

Influence of Soda and Kraft lignin in polyurethane coatings for the corrosion protection of mild steel in 3.5 % NaCl solution

This study highlights the potential of coconut shell biomass waste-derived lignins (CSL) as corrosion inhibitors to reinforce the coating properties of polyurethane. The utilization of CSL involves a green approach to prepare eco-friendly metallic coatings. Herein, lignin was extracted via Kraft and Soda pulping processes. The present findings indicated that the percentage yield of Soda lignin (SL) (26.43 ± 0.75 %) was significantly higher than that of Kraft lignin (KL) (8.52 ± 0.39 %). Electrochemical impedance spectroscopy and potentiodynamic polarization corrosion monitoring techniques were used to evaluate the anticorrosive performance of modified polyurethane coatings on mild steel exposed to 3.5 % NaCl solution. In this study, doping concentration of 5 wt% KL and SL into polyurethane attained the optimum anticorrosion performance. The surface conditions of uncoated and coated mild steel substrates were investigated through scanning electron microscopy/energy dispersive X-ray (EDX) analysis, salt spray and adhesion tests. EDX analysis demonstrated that polyurethane added with 5 wt% doping concentration of SL contained the highest content of Fe (86.05 wt%) compared to 5 wt% KL which contained 79.64 wt% of Fe, whereas neat polyurethane coating contained 75.43 wt% of Fe. Hence, enhanced corrosion protection of polyurethane through the addition of CSL, particularly SL, possesses a viable and an effective green approach to utilize coconut shell biomass waste for the application as a potential corrosion inhibitor in organic coatings.

Assessment of the Influence of Fabric Structure on Their Electro-Conductive Properties.

Electro-conductive fabrics are key materials for designing and developing wearable smart textiles. The properties of textile materials depend on the production method, the technique which leads to high conductivity, and the structure. The aim of the research work was to determine the factors affecting the electrical conductivity of woven fabrics and elucidate the mechanism of electric current conduction through this complex, aperiodic textile material. The chemical composition of the material surface was identified using scanning electron microscopy energy dispersion X-ray spectroscopy. The van der Pauw method was employed for multidirectional resistance measurements. The coefficient was determined for the assessment of the electrical anisotropy of woven fabrics. X-ray micro-computed tomography was used for 3D woven structure geometry analysis. The anisotropy coefficient enabled the classification of electro-conductive fabrics in terms of isotropic or anisotropic materials. It was found that the increase in weft density results in an increase in sample anisotropy. The rise in thread width can lead to smaller electrical in-plane anisotropy. The threads are unevenly distributed in woven fabric, and their widths are not constant, which is reflected in the anisotropy coefficient values depending on the electrode arrangement. The smaller the fabric area covered by four electrodes, the fewer factors leading to structure aperiodicity.

Development of red mud based sintered artificial aggregates with various industrial wastes

Red mud (RM) has drawn a lot of attention in the search for potential uses in the production of sintered artificial aggregate from industrial waste products. The main objective of the study is to produce an RM-based sintered artificial aggregate (SAA), with several blends (binary, ternary, and quaternary) using various industrial wastes. This study includes assessing the mechanical and physical properties of SAA as well as the sintering parameters in order to determine the appropriate material mix ratio. To achieve these objectives, a comprehensive experimental approach was adopted. A total of 35 different mixtures were formulated by incorporating various industrial wastes as binders and sintering additives. The green pellets were preheated at 105 °C for 24 h, and consecutively sintered at different temperatures, namely 700 °C, 900 °C, 1100 °C, and 1150 °C with a duration of 30 min. A compressive strength test was performed in order to find the mechanical property of SAA similarly water absorption and bulk density tests were conducted to find the physical properties of SAA. To characterize the SAA, scanning electron microscope analysis (SEM), X-ray diffraction (XRD) and energy dispersive x-ray analysis were conducted, and also data analysis was performed using Artificial Neural Network (ANN) tools, yielding accurate predictions. Successfully best compressive strength low water absorption SAA was produced. The best material weight mix ratio for the production of SAA was identified as (A18) RM: Fly Ash: Waste Glass Powder; 78:10:12. Out of all blends the ternary blend (A18) SAA exhibited impressive properties after 30 min of sintering at 1150 °C: high compressive strength of 22.92 MPa, water absorption of 4.26%, and bulk density of 1296.12 kg m−13. This was made possible by the high amount of Al2O3, SiO2, in the combination of fly ash, and waste glass powder with RM. SEM and XRD analysis also confirmed that the (A18) SAA achieved the best compressive strength, and low water absorption due to turning the surface and core area into a solid, reduced internal pores and formed quartz, and hematite phases. The findings of this study serve as a foundation for future work and pave the way for the development of sustainable construction materials.

Novel starch–tungsten (VI) oxide biocomposites: Preparation, characterization, and comparisons between experimental and theoretical photon attenuation coefficients

This study synthesized biocomposites containing starch and WO3 at varying ratios of 10 %, 20 %, 30 %, 40 %, and 50 % and assessed their thermal and radiation-shielding properties. These biocomposites were characterized using Fourier-transform infrared spectroscopy, X-ray diffraction (XRD) analysis, particle-size distribution assessments, scanning electron microscopy–energy dispersive X-ray spectroscopy, and thermogravimetric analysis–differential thermogravimetry measurements. Furthermore, the linear attenuation coefficients of the biocomposites were experimentally measured using an NaI(Tl) gamma spectrometry system and theoretically computed using XCOM and GAMOS simulations for comparisons. The XRD and particle-size distribution profiles of the WO3.2H2O powder, respectively, demonstrated evident diffraction peaks and favorable pore-size distributions. Morphological characterizations revealed that the WO3 particles were homogeneously dispersed throughout the starch matrix without any agglomeration. Comparisons of the thermal degradation rates revealed that the pure starch and starch +50%WO3 biocomposite began decomposing at approximately 200°Cand 300 °C, respectively, indicating that increasing WO3 proportions enhanced thermal stability. Furthermore, the starch +50%WO3 biocomposite demonstrated the highest experimental linear attenuation coefficient, with a value of 0.2510 ± 0.0848 cm−1 at a gamma energy of 662 keV. Meanwhile, XCOM and GAMOS simulations revealed theoretical attenuation coefficients of 0.1229 and 0.1213 cm−1 for pure starch and 0.2202 cm−1 and 0.2178 cm−1 for the starch +50%WO3 biocomposite at 662 keV, respectively.

Green Synthesis of Copper Nanoparticles Using Polyalthia longifolia Roots and their Bioactivities Against Escherichia coli, Staphylococcus aureus, and Candida albicans

ABSTRACT The synthesis of copper nanoparticles (CuNPs) has been the center of researchers’ attention due to their potential in various fields, particularly in medicine and pharmacy. The objective of this research was to synthesize CuNPs by using the extract from Polyalthia longifolia roots via an organic solvent-free approach. The roots of P. longifolia were extracted using boiling water and subsequently used to synthesize CuNPs from CuSO4 solution. The resultant nanoparticles were then characterized using UV–Vis spectrophotometer, Fourier transform infrared (FTIR), X-ray diffraction (XRD), scanning electron microscope–energy dispersive X-ray (SEM-EDX), and transmission electron microscopy (TEM). Kirby–Bauer sensitivity test was performed against Staphylococcus aureus, Escherichia coli, and Candida albicans. In the results, we found that the total phenolic content and total flavonoid content of the extract were 85.43 GAE/g dry extract and 0.78 QE/g dry extract, respectively. The characterizations revealed that the obtained nanoparticles possess a spherical shape and diameters of around 2 to 10 nm. The XRD suggests that the nanoparticles were occupied by copper (0) and copper oxides (CuO, CuO2, and Cu2O). The synthesized CuNPs yielded inhibition zones of 17.2 ± 0.2, 15.6 ± 0.2, and 13.7 ± 0.1 mm against S. aureus, E. coli, and C. albicans, respectively. In conclusion, aqueous extract from the roots of P. longifolia can be used to synthesize CuNPs that could be used as an antibacterial and antifungal agent.

Characterization of an advanced bone graft material with a nanocrystalline hydroxycarbanoapatite surface and dual phase composition.

The bone formation response of ceramic bone graft materials can be improved by modifying the material's surface and composition. A unique dual-phase ceramic bone graft material with a nanocrystalline, hydroxycarbanoapatite (HCA) surface and a calcium carbonate core (TrelCor®-Biogennix, Irvine, CA) was characterized through a variety of analytical methods. Scanning electron microscopy (SEM) of the TrelCor surface (magnification 100-100,000X) clearly demonstrated a nanosized crystalline structure covering the entire surface. The surface morphology showed a hierarchical structure that included micron-sized spherulites fully covered by plate-like nanocrystals (<60 nm in thickness). Chemical and physical characterization of the material using X-ray Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR), and Scanning Electron Microscopy Energy Dispersive X-ray Spectroscopy (SEM-EDX) showed a surface composed of HCA. Analysis of fractured samples confirmed the dual-phase composition with the presence of a calcium carbonate core and HCA surface. An in vitro bioactivity study was conducted to evaluate whether TrelCor would form a bioactive layer when immersed in simulated body fluid. This response was compared to a known bioactive material (45S5 bioactive glass - Bioglass). Following 14-days of immersion, surface and cross-sectional analysis via SEM-EDX showed that the TrelCor material elicited a bioactive response with the formation of a bioactive layer that was qualitatively thicker than the layer that formed on Bioglass. An in vivo sheep muscle pouch model was also conducted to evaluate the ability of the material to stimulate an ectopic, cellular bone formation response. Results were compared against Bioglass and a first-generation calcium phosphate ceramic that lacked a nanocrystalline surface. Histology and histomorphometric analysis (HMA) confirmed that the TrelCor nanocrystalline HCA surface stimulated a bone formation response in muscle (avg. 11% bone area) that was significantly greater than Bioglass (3%) and the smooth surface calcium phosphate ceramic (0%).

Atomic-level investigation of structure and formation process of Y3Al5O12 with super-high content of Ce emitting anomalous orange-red emissions

Ce-doped yttrium aluminum garnet (YAG:Ce, Y3Al5O12:Ce) is the most commonly used yellow phosphor in white light-emitting diodes. Recently, we found that (Y1–xCex)3Al5O12:Ce with a super-high content of Ce (x = 0.11–0.21) can be prepared by a polymerized complex method and exhibits anomalous orange–red emission. To understand the nature of this anomalous behavior from the atomic level, we applied high-angle annular dark-field scanning transmission electron microscopy (HAADF-STEM) and scanning transmission electron microscopy–energy dispersive X-ray spectroscopy (STEM-EDS), a state-of-the-art technique that enables analysis of the atomic-level elemental distributions of Al, Y, and Ce. STEM-EDS images on the atomic level were successfully obtained for YAG:Ce. It was found that Ce in Y site has spatially uneven for few nanometers. Ce–K edge extended X-ray absorption fine structure (EXAFS) analysis was also conducted, which revealed a high level of asymmetry around Ce. By combining the STEM-EDS and EXAFS results, a dynamic model for the red emission was proposed. STEM-EDS also revealed that CeO2 nanocrystals were firstly formed with low-temperature annealing and that the reaction of Y with the CeO2 nanocrystals subsequently yielded YAG:Ce, unlike in the conventional one-step high-temperature synthesis.

Influence of TiO2 Nanoparticles on the Physical, Mechanical, and Structural Characteristics of Cementitious Composites with Recycled Aggregates.

The aim of this study is to analyze the effect of the addition of TiO2 nanoparticles (NTs) on the physical and mechanical properties, as well as the microstructural changes, of cementitious composites containing partially substituted natural aggregates (NAs) with aggregates derived from the following four recycled materials: glass (RGA), brick (RGB), blast-furnace slag (GBA), and recycled textolite waste with WEEE (waste from electrical and electronic equipment) as the primary source (RTA), in line with sustainable construction practices. The research methodology included the following phases: selection and characterization of raw materials, formulation design, experimental preparation and testing of specimens using standardized methods specific to cementitious composite mortars (including determination of apparent density in the hardened state, mechanical strength in compression, flexure, and abrasion, and water absorption by capillarity), and structural analysis using specialized techniques (scanning electron microscopy (SEM) images and energy dispersive X-ray spectroscopy (EDS)). The analysis and interpretation of the results focused primarily on identifying the effects of NT addition on the composites. Results show a decrease in density resulting from replacing NAs with recycled aggregates, particularly in the case of RGB and RTA. Conversely, the introduction of TiO2 nanoparticles resulted in a slight increase in density, ranging from 0.2% for RTA to 7.4% for samples containing NAs. Additionally, the introduction of TiO2 contributes to improved compressive strength, especially in samples containing RTA, while flexural strength benefits from a 3-4% TiO2 addition in all composites. The compressive strength ranged from 35.19 to 70.13 N/mm2, while the flexural strength ranged from 8.4 to 10.47 N/mm2. The abrasion loss varied between 2.4% and 5.71%, and the water absorption coefficient varied between 0.03 and 0.37 kg/m2m0.5, the variations being influenced by both the nature of the aggregates and the amount of NTs added. Scanning electron microscopy (SEM) images and energy dispersive X-ray spectroscopy (EDS) analysis showed that TiO2 nanoparticles are uniformly distributed in the cementitious composites, mainly forming CSH gel. TiO2 nanoparticles act as nucleating agents during early hydration, as confirmed by EDS spectra after curing.

Development of suitable magnetite–diatomite nanocomposite for Cd (II) adsorptive removal from wastewater

A magnetite-diatomite nanocomposite (MDM) adsorbent was synthesized using the co-precipitation method, wherein a magnetite precursor was intercalated into diatomite clay minerals sourced from the Ethiopian Rift Valley. Fourier-transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), scanning electron microscopy energy dispersive x-ray (SEM-EDX), Brunauer-Emmett-Teller (BET) and magnetometry measurements were used to look into the structure and magnetic properties of the adsorbent. Batch experiments were conducted to study the remarkable Cd (II) adsorption capacity of MDM and the ease of separating the used adsorbent with a bar magnet. The most important adsorption parameters, namely, initial pH, adsorbent dose (g), initial (Cd (II) concentration (mg), and contact time (min), were optimized using Box-Behnken design (BBD). The MDM has shown exceptional Cd (II) removal under optimum conditions, with a maximum adsorption capacity of 31.4 mg/g from aqueous solution. Based on the results of isotherm and kinetic studies, the Temkin and pseudo-second-order models were found to provide the most accurate fit for adsorption equilibrium when compared to the alternative models. The thermodynamic studies, under standard conditions revealed that, Cd (II) uptake is exothermic and spontaneous. The finding of this study confirms that the MDM adsorbent is easily reusable, extractable from the solution using an external magnet, and capable of recovering around 80 % of Cd (II) when HNO3 is used as a desorbing agent. The study demonstrates a cost-effective and environmentally friendly approach to remediate Cd (II) pollution in wastewater. Furthermore, the superior Cd (II) adsorption capacity, combined with the ease of separating using a bar magnet and high reusability, highlights the potential of this novel adsorbent as a sustainable and efficient solution for addressing Cd (II) contamination in various wastewater treatment applications.Thereby contributing significantly to advancements in the field of heavy metal removal from aqueous solutions.

A comprehensive characterization of indoor ambient microplastics in households during the COVID-19 pandemic

AbstractAirborne microplastics (MPs) can be easily inhaled by humans, impacting their health as they spend more than 80% of their time indoors, especially during the pandemic. Only a few research studies have examined indoor MPs in the micrometer size range using active sampling, and studies have mainly concentrated on MPs that are millimeters in size. This study investigated the composition of indoor airborne MPs by active sampling in seven houses in the city center of northwestern Turkey (Eskişehir) during the COVID-19 pandemic. The visual identification showed the presence of different colored MPs, white, red, orange, green, and yellow, with different shapes (fibers, fragments, films, lines, foam, and pellets). The size of the identified MPs was between 2.5 and 327.36 μm. The polymeric composition analysis showed the presence of 123 MPs in all the samples with 22 different polymeric compositions. Residents in these houses are exposed to airborne MPs, with inhalation estimates ranging from 12.03 to 18.51 MPs/m3. However, it was also estimated that humans inhale 156–240 MPs daily in these houses. The dominant MPs were polyamide 6, polyvinyl chloride, polypropylene, ethylene propylene, polystyrene, and high-density polyethylene. Scanning electron microscopy energy dispersive x-ray elemental analysis revealed the presence of common structural elements, additives, or vectors that are added or adsorbed to MPs like carbon, oxygen, fluorine, magnesium, silicon, chlorine, nitrogen, and aluminum. These indoor environments are prone to MP pollution. Still, the MP level varies due to different characteristics of indoor environments, like activities and the number of occupants/people in the space, etc. The smaller MPs in all the samples highlight the necessity for standardized techniques of MP collection.

On dry machining of AZ31B magnesium alloy using textured cutting tool inserts

Magnesium alloys have many advantages as lightweight materials for engineering applications, especially in the fields of automotive and aerospace. They undergo extensive cutting or machining while making products out of them. Dry cutting, a sustainable machining method, causes more friction and adhesion at the tool-chip interface. One of the promising solutions to this problem is cutting tool surface texturing, which can reduce tool wear and friction in dry cutting and improve machining performance. This paper aims to investigate the impact of dimple textures (made on the flank face of cutting inserts) on tool wear and chip morphology in the dry machining of AZ31B magnesium alloy. The results show that the cutting speed was the most significant factor affecting tool flank wear, followed by feed rate and cutting depth. The tool wear mechanism was examined using scanning electron microscope (SEM) images and energy dispersive X-ray spectroscopy (EDS) analysis reports, which showed that at low cutting speed, the main wear mechanism was abrasion, while at high speed, it was adhesion. The chips are discontinuous at low cutting speeds, while continuous at high cutting speeds. The dimple textured flank face cutting tools facilitate the dry machining of AZ31B magnesium alloy and contribute to ecological benefits.

Synthesis and Characterization of Carbonate Hydroxyapatite from Pokea Clam Shells (&lt;i&gt;Batissa Violacea Var. Celebensis&lt;/i&gt;) by Precipitation and Hydrothermal Methods

Hydroxyapatite Carbonate (CHA) is a material that is found to have a composition more similar to bone, with a higher bioactivity than Hydroxyapatite (HA). CHA was synthesized using precipitation and hydrothermal methods using (NH4)2HPO4 as a phosphate source, NH4HCO3 as a carbonate source, and Pokea shells as a calcium source. In this study, the Pokea shells were crushed, calcined, and characterized based on physicochemical tests. CaO from Pokea shell contains 74.33% calcium. CHA was successfully produced by precipitation method at room temperature and hydrothermal at 120 C for 8 h. Sample characterization was carried out using X-Ray Diffraction (XRD), Fourier Transform Infrared (FTIR), and Scanning Electron Microscope Energy Dispersive X-Ray Spectroscopy (SEM-EDX). Based on XRD data, there are differences in the crystal size of CHA produced via precipitation and hydrothermal methods, where the crystal sizes of Precipitation CHA-1 and Hydrothermal CHA-2 are 6.388 nm and 25.969 nm. The FTIR results of both CHA show the functional groups typical of CHA, namely OH-, CO, CaO, PO43-, and CO32-. From the Ca/P EDX data results, Precipitation CHA-1 and Hydrothermal CHA-2 do not differ much, namely 1.71 and 1.69, and this value indicates that CHA has been formed.

Characterization of Tableware from Fábrica de Loiça de Sacavém—Linking Analytical and Documental Research

Fábrica de Loiça de Sacavém (ca. 1858–1994) was among the first to produce white earthenware in Portugal, becoming one of the country’s leading ceramic manufacturers during the late 19th to early 20th centuries. Research on white earthenware has accompanied the growing interest in post-industrial archaeology but is still poorly explored compared to more ancient ceramic productions. This study focused on the ceramic body, glazes, and colourants of tableware produced by Fábrica de Loiça de Sacavém during the first 50 years of its activity (1859–1910). A multi-analytical approach was selected to investigate the chemical and mineralogical composition of the ceramic body, glaze, and pigments using optical microscopy, variable-pressure scanning electron microscope energy-dispersive X-ray spectroscopy (VP-SEM-EDS), μ-Raman spectroscopy, μ-X-ray Diffraction (μ-XRD), and reflectance spectroscopy (hyperspectral image analysis). The studied tableware was produced with a Ca-poor siliceous–aluminous white earthenware ceramic body covered with transparent alkali lead or lead borosilicate glaze, and most colourants were complex Cr-based pigments. These results are in agreement with the little documental evidence from this period found in the manufacturer’s archives.

Characterization of Mn5Ge3 Contacts on a Shallow Ge/SiGe Heterostructure.

Mn5Ge3 is a ferromagnetic phase of the Mn-Ge system that is a potential contact material for efficient spin injection and detection. Here, we investigate the creation of Mn5Ge3-based contacts on a Ge/SiGe quantum well heterostructure via solid-state synthesis. X-ray diffraction spectra fitting indicates the formation of Mn5Ge3-based contacts on bulk Ge and Ge/SiGe. High-resolution scanning transmission electron microscopy imaging and energy dispersive X-ray spectroscopy verify the correct Mn5Ge3-based phase formation. Schottky diode measurements, transmission line measurements, and Hall measurements reveal that Mn5Ge3-based contacts serve as good p-type contacts for Ge/SiGe quantum well heterostructures due to having a low Schottky barrier height of 0.10eV (extracted from a Mn5Ge3/n-Ge analogue) and a contact resistance in the order of 1 kΩ. Furthermore, we show that these electrical characteristics have a gate-voltage dependence, thereby providing tunability.

Long-term corrosion of copper alloys in the soil: new aspects of corrosion morphology in archaeological vessels from south-western Iran

A group of copper-based objects excavated at Deh Dumen cemetery, in south-western Iran, was studied and analysed to examine the long-term corrosion morphology and mechanism in the soil burial environment. For this purpose, twenty-two samples from twenty-one copper-based vessels were studied and analysed using X-ray diffraction, scanning electron microscopy—energy dispersive X-ray spectroscopy, micro-Raman spectroscopy and metallography techniques. The results of the analyses showed that the majority of vessels are made of tin bronze, along with two arsenical copper samples. The extent of corrosion observed ranges from very thin corrosion crusts to thick crusts and entirely corroded structures. These three identified corrosion morphologies display a multi-layered corrosion stratigraphy as well as the preserved limit of the original surface. The corrosion crusts include internal tin-rich and external copper-rich layers, and the main corrosion mechanism for the formation of multi-layered corrosion crusts is decuprification or selective dissolution of copper during the long-term burial time in a moderately Cl-contaminated soil. The three identified corrosion morphologies are similar to the previously published morphologies, but some clear deviations are apparent and are discussed here.

Selective recovery of rare earth elements by smelting of magnets

Rare earth elements (REEs) play a crucial role in many technologies from daily appliances in cell phones to more advanced wind turbines and electric cars. Permanent magnets account for a quarter of total global REEs production and have high recycling value. In this study, smelting process was used to selectively oxidize REEs in the permanent magnets by adding Fe2O3. This separates REEs into a slag phase from an iron-rich metallic phase. B2O3 was also added to the system as a flux to lower the slag melting temperature. This minimizes REEs loss to the metallic phase and allows a more efficient phase separation. The effect of flux and oxidizing agent addition was investigated on both regular and cerium-rich NdFeB (NdCeFeB) magnets. At 1350 °C and for 1 h, the slag phase was successfully separated from the metallic phase with the addition of 0.8 stoichiometric amount of Fe2O3 and 40 wt% of B2O3. Scanning electron microscopy–energy dispersive X-ray spectroscopy (SEM-EDX) analysis reveals that REEs in the magnet do not migrate to the metal phase while the REE-rich slag phase contains almost no iron. After the selective removal of iron into the metallic phase, REEs are recovered from the slag phase through an acid leaching process allowing >99% of REEs recovery. Boron in the magnet can also be recovered as useful boric acid by evaporation and crystallisation technique. The proposed process in this study is reagent and energy-efficient with almost complete valorisation of both NdCeFeB and NdFeB magnets.