Electron Microscopy-energy Dispersive Spectroscopy Research Articles

Engineered K-doped ZnO/borneol based hydrogel composite material for led-based photocatalytic degradation of methylene blue and evaluation of antimicrobial activity

The significant improvement of decolorization and disinfection technologies has been a hotspot in wastewater reutilization. In this study, we realized a novel construction of K-doped nano-ZnO and borneol based hydrogel composite material (K-ZnO/B-hydrogel) by low-temperature in situ sol–gel growth. The techniques such as fourier transform infrared (FTIR), X-ray diffraction (XRD), x-ray photoelectron spectroscopy (XPS), scanning electron microscope (SEM) and X-ray energy dispersive spectroscopy (EDS) were applied to recognize the synthesized hydrogel. The results revealed that K-doped ZnO nanoparticles had been uniformly decorated onto the B-hydrogel. Ultraviolet-visible (UV–vis) absorption spectra showed that impurity doping of potassium element into ZnO could reduce the band gap, improving the visible light absorption efficiency. Under LED illumination, the photodegrading rate of K-ZnO/B-hydrogel was approximately 2.3 times greater than that of K-ZnO/B-hydrogel on methylene blue (MB) removal. Remarkably, aside from CO2 and H2O, no by-products were generated during the photodegradation process. In addition, the antimicrobial activities against Escherichia coli (E. coli) and Staphylococcus aureus (S. aureus) of K-ZnO/B-hydrogel achieved up to 99.9%, which were at least 1.5 times higher than K-ZnO/B-hydrogel. This composite will push ahead with a closed-loop wastewater treatment system for dye and pathogenic microorganism disposal, which combines the excellent adsorption ability of hydrogel and the outstanding photocatalytic ability of ZnO nanoparticles with easy sample handling and separation, and help to eliminate secondary pollution.

Electrochemical high sensitive detection of hydrogen peroxide based on platinum-palladium nano-enzyme modified microelectrode

Hydrogen peroxide (H2O2) is widely distributed in living organisms and the environment, and its concentration is closely associated with human health. Therefore, the development of an efficient and sensitive detection method for H2O2 is imperative. In this study, a PtPd nano-enzyme composite was electrodeposited onto a platinum wire microelectrode (ME) using a one-step electrochemical deposition method to fabricate an H2O2 electrochemical sensor (PtPd/ME) with exceptional performance. The successful modification of PtPd on the electrode surface was confirmed by scanning electron microscopy (SEM) and X-ray energy dispersive spectroscopy (EDS). Chronoamperometry (i-t) was employed to investigate various technical parameters including sensitivity, detection limit, detection range, reproducibility, and anti-interference capability. The results demonstrate that the sensor exhibits a sensitivity of 11.94 mA M-1 cm-2 with a detection limit of 0.034 μM and a wide linear range from 31.25 μM to 4.15 mM while also demonstrating excellent anti-interference properties. These superior performances can be attributed to the strong catalytic activity towards H2O2 provided by PtPd nanoparticles as well as the fast electron transfer rate facilitated by microelectrodes. Furthermore, this sensor effectively enables real-time monitoring of H2O2 released by ascorbic acid-stimulated vascular endothelial cells and demonstrates its potential for detecting H2O2 in contact lens care solutions. These findings provide valuable insights for food and drug testing, and demonstrate great potential for monitoring key pathological processes within living cells.

Investigations of In2O3 Added SiC Semiconductive Thin Films and Manufacture of a Heterojunction Diode

This study involved direct doping of In2O3 into silicon carbide (SiC) powder, resulting in 8.0 at% In-doped SiC powder. Subsequently, heating at 500 °C was performed to form a target, followed by the utilization of electron beam (e-beam) technology to deposit the In-doped SiC thin films with the thickness of approximately 189.8 nm. The first breakthrough of this research was the successful deposition of using e-beam technology. The second breakthrough involved utilizing various tools to analyze the physical and electrical properties of In-doped SiC thin films. Hall effect measurement was used to measure the resistivity, mobility, and carrier concentration and confirm its n-type semiconductor nature. The uniform dispersion of In ions in SiC was as confirmed by electron microscopy energy-dispersive spectroscopy and secondary ion mass spectrometry analyses. The Tauc Plot method was employed to determine the Eg values of pure SiC and In-doped SiC thin films. Semiconductor parameter analyzer was used to measure the conductivity and the I-V characteristics of devices in In-doped SiC thin films. Furthermore, the third finding demonstrated that In2O3-doped SiC thin films exhibited remarkable current density. X-ray photoelectron spectroscopy and Gaussian-resolved spectra further confirmed a significant relationship between conductivity and oxygen vacancy concentration. Lastly, depositing these In-doped SiC thin films onto p-type silicon substrates etched with buffered oxide etchant resulted in the formation of heterojunction p-n junction. This junction exhibited the rectifying characteristics of a diode, with sample current values in the vicinity of 102 mA, breakdown voltage at approximately −5.23 V, and open-circuit voltage around 1.56 V. This underscores the potential of In-doped SiC thin films for various semiconductor devices.

Automated SEM analysis of particles in Hanford tank waste

Multiple bench-scale filtration campaigns of Hanford tank waste supernatant on a backpulseable dead-end filtration skid have provided greater insight into the solids that cause fouling and reduce filter performance. The solids collected during each campaign were concentrated from the backpulse solutions and examined using automated particle analysis (APA) methods with scanning electron microscopy and X-ray energy dispersive spectroscopy to categorize particle types and their morphological characteristics. We show that with APA, thousands of particles can be analyzed to provide accurate insight into the phases that may be impacting filter performance.

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.

Preparation and fluorescence detection of nitrogen-doped carbon quantum dots/cotton fiber composites

From the perspective of environmental protection and sustainable development, fluorescent probes have been prepared using inexpensive raw materials for fluorescence detection in wastewater treatment. Nitrogen-doped carbon quantum dots (N-CQDs)/cotton fiber composites were prepared by grafting N-CQDs onto the oxidized cotton fibers using a silane coupling agents. Through a series of characterizations using X-ray photoelectron spectroscopy (XPS), Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM) and X-ray energy dispersive spectrometry (EDS), it was found that N-CQDs were loaded onto cotton fibers. In the N-CQDs/cotton fiber composite, the fluorescence rate of carbon quantum dots is higher, which is 17.2 %, and the detection limit is 1.21 μM. The optimum conditions for fluorescence detection of azo dye Chrome black T(EBT) with pH 8 and concentration 10 μM were studied. This method for the detection of EBT has advantages such as high sensitivity, simplicity, speed, reusability, and a high potential for application in wastewater detection.

Effects of pyrite, quartz and sodium sulfite on roasting of a refractory sulfide concentrate and gold, silver, copper leaching during cyanidation

The oxidation roasting pretreatment process, which is a mature and dominant industrial practice for treating complex polymetallic gold deposits, has a low recovery of associated silver and exhibits an unclear reaction sequence. This study takes a silver-containing gold ore as the research object and investigates the effect of (i) sodium sulfite as an additive, (ii) main gold-bearing mineral pyrite, and (iii) gangue mineral quartz, on silver during the roasting process in roasting and leaching tests. Characterization techniques included scanning electron microscopy–energy dispersive spectroscopy analysis, and thermogravimetry–differential scanning calorimetry analysis. The results based on thermodynamic calculations and characterization show that the main reason for the low extraction of silver is that the calcined product (i.e., iron silicate) formed by the reaction between pyrite and quartz during the roasting process is mutually absorbed and wrapped with silver oxide. In addition, silver minerals decompose some iron sulfides and iron oxides under high-temperature conditions, promoting the reaction of iron and quartz to form iron silicate while strengthening the secondary encapsulation of silver by products of roasting, thus deteriorating the extraction of silver. The addition of sodium sulfite reduces the formation of iron silicate and increases the extraction of silver by directly promoting the conversion of pyrite to iron oxide. This study provides a theoretical basis for further improving the roasting and leaching of silver.

Effect of ligand interactions within modified granular activated carbon (GAC) on mixed perfluorooctanoic acid (PFOA) and perfluorooctanesulfonic acid (PFOS) adsorption

A new adsorbent based on commercial granular activated carbon (GAC) and loaded with Cu(II) (GAC-Cu) was prepared to enhance the adsorption capacity of perfluorooctanoic acid (PFOA) and perfluorooctane sulfonate (PFOS). The surface area (SA) and pore volume of GAC-Cu decreased by ∼15% compared to those of pristine GAC. The scanning electron microscopy–energy dispersive spectrometry (SEM-EDS) and leaching test results indicated that, compared with GAC, the Cu atomic ratio and Cu amount in GAC-Cu increased by 2.91 and 2.43 times, respectively. The point of zero charge (PZC) measured using a salt addition method obtained a pH of 6.0 (GAC) and 5.0 (GAC-Cu). According to the isotherm models obtaining highest coefficient of determination (R2), GAC-Cu exhibited a 20.4% and 35.2% increase for PFOA and PFOS in maximum uptake (qm), respectively, compared to those of GAC. In addition, the adsorption affinity (b) for GAC-Cu increased by 1045% and 175% for PFOA and PFOS, respectively. The pH effect on the adsorption capacity of GAC-Cu was investigated. The uptake of PFOA and PFOS decreased with an increase in pH for both GAC and GAC-Cu. GAC-Cu exhibited higher uptake than GAC at pH 6 and 7, but no enhanced uptake was observed at pH 4.0, 5.0, and 8.5. Therefore, ligand interaction was effective at weak acid or neutral pH.

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 (<i>Batissa Violacea Var. Celebensis</i>) 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 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.

The Corrosion Resistance of Concrete-Filled Steel Tubes with the Assembly Unit of Na2MoO4 and Benzotriazole

Steel pipes are commonly used to strengthen the concrete’s load-bearing capacity. However, they are prone to corrosion in salt erosion environments. In this study, the influence of Na2MoO4 and benzotriazole on concrete-filled steel tubes’ corrosion performance is investigated. The steel pipes’ mass loss rates (MRs), ultrasonic velocity, electrical resistance, and the AC impedance spectrum and Tafel curves of concrete-filled steel tubes were used to characterize the degree of corrosion in the steel pipes. Scanning electron microscopy–energy-dispersive spectrometry and X-ray diffraction were used for studying the composition of steel pipe rust. The research results revealed that the NaCl freeze–thaw cycles (F-C) and NaCl dry–wet alternation (D-A) actions had a reducing effect on the mass and ultrasonic velocity of the concrete-filled steel tubes. After 300 NaCl F-C and 30 NaCl D-A, the MRs were 0%~0.00470% and 0%~0.00666%. The corresponding ultrasonic velocities were 0%~21.1% and 0%~23.6%. When a rust inhibitor was added, the results were the opposite. The MRs decreased by 0%~80.3% and 0%~81.6% with the added Na2MoO4 and benzotriazole. Meanwhile, the corresponding ultrasonic velocities were 0%~8.1% and 0%~8.3%. The steel tubes were corroded after 300 NaCl F-C and 30 NaCl D-A. The addition of rust inhibitors improved the corrosion resistance of the concrete-filled steel tubes by increasing the electrical resistance before NaCl erosion. The corrosion area rate decreased by using the rust inhibitors. The corrosion resistance effect of benzotriazole was higher than that of Na2MoO4. The concrete-filled steel tube with an assembly unit comprising 5 kg/m3 of Na2MoO4 and 15 kg/m3 of benzotriazole had the best corrosion resistance under the erosion induced by NaCl F-C and D-A. Rust inhibitors reduced the content of iron-containing crystals and iron elements. The specimens with 5 kg/m3 Na2MoO4 and 15 kg/m3 benzotriazole had the lowest concentration of iron-containing crystals and iron elements.

Microbiologically influenced corrosion can cause a dental implant rejection

In the present study, we apply electrochemical and molecular biology approaches to establish whether microbiologically influenced corrosion (MIC) may be the reason for dental implant rejection. Titanium-based implants have been incubated in vitro in Ringer/glucose solution in the presence and absence of a salivary microbiota and the change in their corrosion potential and current density was monitored over time by potentiodynamic polarization. The charge transfers processes occurring on the Ti-based implant surface during the initial bacterial adhesion and after biofilm formation were analyzed by electrochemical impedance spectroscopy. The components of the equivalent electrical circuit as well as the heterogeneous electron transfer rate constants were estimated. In parallel, bacterial species from the salivary microbiota have been identified by sequencing of the 16S ribosomal amplicon method, and their contribution to the corrosion processes of dental implants was verified and compared to that of native saliva in vitro. The scanning electron microscopy observation and energy dispersive spectroscopy analysis of the implant surface after long-term exposure to a bacterial-containing environment revealed more detailed features of the occurring corrosion processes.

In-Line Co-Processing of Stainless Steel Pickling Sludge Using Argon Oxygen Decarburization Slag Bath: Behavior and Mechanism

Stainless steel pickling sludge (SSPS) is classified as hazardous solid waste, while Argon Oxygen Decarburization (AOD) slag is challenging to utilize due to the leaching toxicity of Cr. This study introduces a novel in-line co-processing technique for AOD slag and SSPS, parallel to the steelmaking process, aimed at metal recovery, sulfur fixation, and slag detoxification: pre-treatment-AOD slag bath approach. The transformations and migrations of sulfur and metal elements, such as Fe and Cr, in the co-processed mixture were analyzed using thermogravimetric–mass spectrometry (TG-MS) and scanning electron microscopy–energy dispersive spectroscopy (SEM-EDS). The results indicated that sulfur in SSPS could be transformed from CaSO4 to CaS under controlled low pre-reduction temperatures (below 800 °C), facilitating its stabilization in the slag and achieving a sulfur fixation rate of over 99%. Metal elements, including iron and chromium, first formed a small portion of spinel (FeCr2O4) during the pre-reduction phase, then Fe-Cr or Fe-Cr-C-based alloy particles were rapidly formed at high temperatures and in the presence of reducers in the slag bath (1550 °C), aggregating and growing spontaneously, ultimately achieving a metal recovery rate of over 95%. Furthermore, a reaction model for SSPS briquettes in the AOD slag bath was established to further reveal the mechanisms of sulfur, iron, and chromium stabilization and migration, thereby providing a basis for the harmless disposal of both materials. The product alloys are expected to be used as additives in stainless steel production, while the harmless slag could be safely utilized in the preparation of cementitious auxiliary materials.

Tracking element-mineral associations with unsupervised learning and dimensionality reduction in chemical and optical image stacks of thin sections

In-situ chemical analysis on thin sections is a cornerstone of geochemical research. Despite massive advances in digital image analysis, the interpretation of such data within the optical petrological context of the thin section has largely remained an analogue task in geochemistry. In this contribution, we registered optical and micro-chemical images from large thin section areas. Chemical datasets from scanning electron microscopy energy dispersive spectrometry (SEM-EDX) and Synchrotron X-ray fluorescence microscopy (S-XFM) were exported from proprietary software. We then evaluated two dimensionality reduction techniques against false-colour images and phase maps to test whether previously unnoticed features became discoverable. Principal component analysis (PCA) and deep sparse autoencoder (DSA) neural networks were used to summarise the multi-channel SEM-EDX and S-XFM into one single red-green-blue (RGB) representation each.Applied to an oceanic gabbro, a cratonic peridotite, and a pelagic limestone, the PCA-based dimensionality reduction was found to produce crisp RGB maps of phases with less noise than false-colour three-element RGB maps. They were registered with optical images to form a simple multi-channel input for pixel-based classification into classes (i.e., semantic segmentation). This was fast and worked well for typical igneous and metamorphic rocks (1–3 h routine). In the chemically quite homogenous limestone, the combined optical and S-XFM PCA input was successfully classified into many phases that were unclassifiable on the conventional SEM-EDX phase map. From the segmented optical and S-XFM PCA map, we exported pixel locations of classified accessory phases back into the original proprietary S-XFM software. This allowed quantification of trace elements whose X-ray peaks were invisible in the original S-XFM quantification.The DSA-based approach yielded phase maps with greater noise, but the technique was very strong at detecting subtle features. In the gabbro sample, the DSA image identified cryptic relict cores in clinopyroxene more clearly than in the previously used Cr concentration map. A DSA training set can be obtained on a small ROI to generate a consistent large area DSA image from which more fragmental cores were observed. For a ROI on the gabbro thin section, the DSA representation map and the blended optical image were segmented and inspected with a loupe tool. This allowed us to generate interactive histograms and bin-scatter concentration plots of selected phases and to search for co-variations of element concentrations. This approach can be expanded to include data from any in situ geochemical acquisition tools and may help discover previously unseen features in complex elemental imagery.

A Bronze Age lip-paint from southeastern Iran

A small chlorite vial, discovered among numerous artifacts looted and recovered in the Jiroft region of Kerman province, southeastern Iran, contains a deep red cosmetic preparation that is likely a lip-coloring paint or paste. Through analytical research involving XRD (X-ray diffraction), SEM–EDS (scanning electron microscopy-energy-dispersive spectroscopy), and HPLC–MS (high-performance liquid chromatography-mass spectrometry) analyses, the mineral components of the reddish substance were identified as hematite, darkened with manganite and braunite, and traces of galena and anglesite, mixed with vegetal waxes and other organic substances. The mixture, thus observed, bears a striking resemblance to the recipes of contemporary lipsticks. We also report the first radiocarbon date ever obtained from a Bronze age cosmetic in the ancient Near East: results place the pigment in the early 2nd millennium BCE, a date compatible with several mentions of the powerful eastern-iranian civilization of Marḫaši in coeval cuneiform texts of Mesopotamia, as well as with its currently emerging archaeological picture.

Synthesis of TiO2/Fe2O3 Nanocomposites as Photocatalyst for Methyl Orange Degradation

Fe2O3/TiO2 composites were successfully synthesized using the sol-gel method. The photocatalytic performance of prepared nanocomposites to degrade methyl orange under UV light irradiation was systematically investigated. The Fe2O3 added and calcination temperature were varied to study their effect on psychochemical properties. Further, to study the effect of psychochemical properties of the prepared nanocomposites on photocatalytic activity, X-ray diffraction (XRD), and scanning electron microscope Energy Dispersive X-ray spectroscopy (SEM-EDS) characterization were conducted. The visible light active Fe2O3 photocatalyst managed to decrease the bandgap energy of the prepared composites from 3.32 eV to 1.95 eV. This decrease in the band gap energy led to the composite being more active under visible light and less active under UV light irradiation. A composite with 6% Fe2O3 content exhibits the smallest degradation efficiency of 14% in 180 min, while the pure TiO2 nanoparticles are 94%. The results in this study provided important implications for further research on the preparation of composite TiO2 with Fe2O3 co-catalyst showing a promising route for improving the visible light activity of photocatalysts.

Failure Modes in Sulfide-Based All Solid-State Batteries (ASSB) Investigated By Operando SEM

Studies on solid state batteries (ASSB) which began back in 190’s has seen a tremendous growing interest for multiple reasons such as the safety and the ability to use the metallic anodes for enhancing the gravimetric energy density. However, it exists different issues linked with poor performance of the batteries, which could be the results of interfacial challenges such as poor ion transport, dendrite formation, electrochemical degradation and chemo-mechanical degradation[1]. Among the potential parameters impacting the cycling process, the influence of the particle size of solid electrolyte is not well studied.In this study, we focused on sulfide-based SEs particle size distribution and its impact on electrochemical performance by investigating from the morphological point of view via operando SEM. A batch of Argyrodite (Li6PS5Cl (LPSCl)) was sieved to obtain two batches of particles range (0,5-20µm and 50-150µm). The AASBs were prepared using the two particles size distribution while keeping the anode (lithium metal), cathode (MA: NMC) composite formation and the fabrication process constant. The different morphological and chemical evolutions were monitored in real time by scanning electron microscopy (SEM) and X-ray energy dispersive spectroscopy (EDX) to obtain a complete of the different modification throughout the battery components and their interfaces. To do so, a home-made electrochemical cell was developed to perform in-situ and operando cycling in the SEM.From the two particles sized distribution, the one with the large particles have better electrochemical performance. From morphological point of view at the cathode composite electrode, the formation of a cathode electrolyte interface is visible in the different batteries but is more developed in the case of small sized particles. In the solid electrolyte, the type of cracks differs with relatively strait feature for small particles and sinuous one for large one. At the anodic interface, a lost in contact between the SE separator and the lithium is observed and increased with the cycling process with a higher impact for the small particles (Figure 1.a and b). By investigating further, the formation of dendrites with different morphologies are visible at the anodic interfaces (Figure1.c).We categorized the observed changes into three modes: (i) electrical failure by the formation of lithium dendrites of different morphologies following the ES going up to short circuit in the case of small particles, (ii) mechanical failure by the formation of cracks in the electrolyte whose shape and propagation strongly depend on the distribution particles size and (iii) electrochemical failure with the formation of solid electrolyte interphases on the surface of the active material. The main obstacles for the use of lithium metal are related to the propagation of lithium dendrites and thus to the mechanical instability of solid electrolytes.

Flotation of lean coal using trisodium citrate dihydrate as a dispersant in the presence of sodium oleate

Flotation is a highly efficient method for purifying low-ash coal particles from high-ash fine slimes. Herein, the dispersion effect of trisodium citrate dihydrate (TCD) on the reduction of slime coating on low-ash lean coal particle surface was studied using flotation tests, scanning electron microscope–energy Dispersive Spectroscopy (SEM–EDS) observation, turbidity measurements, and extended Derjaguin–Landau–Verwey–Overbeek (E-DLVO) calculations. Flotation tests revealed that after adding of 2000 g/t TCD, the yield of clean coal increased by 1.09 % and the ash content of clean coal decreased by 1.45 % with 1000 g/t NaOL at pH 7.0, thereby increasing the combustible recovery and flotation perfect index by 2.50 % and 6.42 %, respectively. The SEM–EDS observation and turbidity measurements indicated that the coating of the high-ash fine slimes on the low-ash coal particle surface was significantly weakened in the presence of 2000 g/t TCD. Furthermore, the E-DLVO calculations verified that the addition of 2000 g/t TCD increased the energy barrier between the low-ash coal particles and high-ash fine slimes, providing theoretical evidence for flotation tests and SEM–EDS observation. Therefore, TCD served as an effective dispersant for the high-ash fine slimes to improve the flotation performance of lean coal.

Brushite/hydroxyapatite coatings on H2SO4 passivated 316LSS by electrodeposition: In vitro corrosion and anti-inflammatory activity

This study evaluated the corrosion behavior and anti-inflammatory activity of brushite (BS or DCPD, CaHPO4·H2O)/hydroxyapatite (HAp, Ca10(PO4)6(OH)2) coating on sulfuric acid (H2SO4) treated 316L stainless steel (SS). The coating was applied using the electrodeposition process on untreated and H2SO4 passivated 316L SS surface. The obtained samples were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM) and X-ray energy dispersive spectroscopy (EDS) to obtain crystal and electronic structure as well as morphological and compositional information of the coated 316L SS. Electrochemical impedance spectroscopy (EIS) tests were performed in 0.9 % sodium chloride (NaCl) solution and compared with the pristine (P316L), H2SO4 treated (T316L), untreated/BS/HAp coated (BHP316L) and treated/BS/HAp coated (BHT316L) 316L SS specimens. The anti-inflammatory activity was carried out for the coated samples by the protein denaturation method. The results showed that the BS/HAp coating on H2SO4 treated 316L SS (hereafter, denoted as BHT316L) were susceptible to corrosion attack against 0.9 % NaCl solution. Additionally, the anti-inflammatory activity of the BHT316L was found to be lower compared to control (sodium diclofenac), indicating that particular concern should be given to H2SO4 treated 316L SS as the corrosion products formed by this surface modification may cause harmful effects in the human physiological environment.