Automated Scanning Electron Microscopy Research Articles

Effect of Ta addition on primary MC carbide in Ti-Nb-Mo-W-alloyed superalloy

The effect of Ta addition on characterization of primary MC carbides with regard to their morphology, composition, and size in Ti-Nb-Mo-W-alloyed Ni-based superalloy were investigated. Several tools including automated scanning electron microscopy as well as electrolytic etching technology were used for broad characterization of carbides including three-dimensional morphology. The addition of Ta significantly influences the composition and morphology of primary MC carbides. Large dendrite (Ti,Nb,W,Mo)C carbides were changed to smaller (Ta,Ti,Nb)C carbides. The hardness of both MC primary carbides and the matrix were increased. MC carbides in the studied superalloys were developed dendrite in three-dimensional morphology, which was much larger than that in two-dimensional morphology. The formation mechanism of carbides was clarified by thermodynamic calculation.

Effect of Silicon–Manganese Deoxidation on Oxygen Content and Inclusions in Molten Steel

In order to improve the cleanliness of steel, non-aluminum deoxidation processes have begun to replace aluminum deoxidation processes. Although the aluminum deoxidation process can reduce the oxygen content in steel to <10 × 10−6, this deoxidation method causes fatigue failure resulting from the formation of large-grained spherical (Ds-type) inclusions composed of calcium–aluminate. It also tends to lead to nozzle blockage during casting. Given the above problems, this study conducted an in-depth investigation of silicon–manganese deoxidation. Thermal experiments and thermodynamic calculations were used to assess the impact of different Mn–Si ratios on the oxygen content and inclusion characteristics during the deoxidation process of molten steel with different initial oxygen contents. The experimental samples were analyzed using an oxygen–nitrogen–hydrogen analyzer, a direct reading spectrometer, and an automatic scanning electron microscope. After that, the samples were electrolyzed to observe the 2D morphology and 3D morphology of the inclusions using scanning electron microscopy. Finally, thermodynamic calculations were carried out using FactSage to verify the experimental results. The results indicated that, regardless of the initial oxygen content, silicon–manganese deoxidation maintained the total oxygen content at 35 × 10−6. It effectively managed the plasticization of inclusions in molten steel, predominantly yielding spherical silicates while minimizing Al-containing inclusions. Nevertheless, as the initial content of [O] increased, the size and density of the silicate inclusions in the steel also increased. An optimal point in the number and size of inclusions was observed with an increased Mn–Si ratio. Moreover, the combined utilization of silicon–manganese deoxidation, diffusion deoxidation, and vacuum deoxidation enabled ultra-low oxygen content control of molten steel.

Mechanical and Microstructural Investigation of Geopolymer Concrete Incorporating Recycled Waste Plastic Aggregate.

The effective use of waste materials is one of the key drivers in ensuring sustainability within the construction industry. This paper investigates the viability and efficacy of sustainably incorporating a polylactic acid-type plastic (WP) as a 10 mm natural coarse aggregate (NA) replacement in geopolymer concrete. Two types of concrete (ordinary Portland cement-OPC and geopolymer) were produced for completeness using a concrete formulation ratio of 1:2:3. The ordinary concrete binder control was prepared using 100% OPC at a water/binder ratio of 0.55, while the geopolymer concrete control used an optimum alkaline activator/precursor-A/P ratio (0.5) and sodium silicate to sodium hydroxide-SS/SH volume ratio (1.2/0.8). Using the same binder quantity as the control, four concrete batches were developed by replacing 10 mm NA with WP at 30 and 70 wt% for ordinary and geopolymer concrete. The mechanical performance of the developed concrete was assessed according to their appropriate standards, while a microstructural investigation was employed after 28 days of curing to identify any morphological changes and hydrated phases. The results illustrate the viability of incorporating WP in geopolymer concrete production at up to 70 wt% replacement despite some negative impacts on concrete performance. From a mechanical perspective, geopolymer concrete indicated a 46.7-58.3% strength development superiority over ordinary concrete with or without WP. The sample composition and texture quantified using automated scanning electron microscopy indicated that adding WP reduced the presence of pores within the microstructure of both concrete types. However, this was detrimental to the ordinary concrete due to the low interfacial zone (ITZ) between calcium silicate hydrate (CSH) gel and WP, resulting in the formation of cracks.

Sulfide Inclusions in an Al‐Killed Nonoriented Electrical Steel with Lanthanum Addition

Herein, laboratory experiments are conducted to evaluate the effect of sulfur and lanthanum content in the steel on the modification of inclusions. The amount, composition, morphology, and size of nonmetallic inclusions in the steel are observed using an automatic scanning electron microscope. Results show that as the lanthanum content in the steel increased from 0 to 72 ppm, the inclusions in the steel with 12 ppm sulfur are modified in the following order: Al2O3–CaO–MgO → LaAlO3 → LaAlO3–La2O2S → La2O2S. Similarly, when the sulfur content is 27 ppm, inclusions transformed in the order of Al2O3–CaO–MgO → LaAlO3 → LaAlO3–La2O2S → La2O2S → La2O2S–LaxS → LaxS as the lanthanum content increases from 0 to 150 ppm. Thermodynamic analysis using FactSage based on a private database is employed to reveal the mechanism for the modification of inclusions. Additionally, a kinetic model is established to study the transformation rate of inclusions in the steel after the addition of lanthanum and sulfur. Liquid Al2O3–CaO–MgO inclusions disappear after 800 s when the steel contains 12 ppm sulfur and 12 ppm lanthanum. The composition of inclusions is 53%LaAlO3–47%La2O2S at 1800 s, while it is 100%La2O2S and 80%La2O2S–18%LaxS–2%CaS when the lanthanum content is 33 and 72 ppm, respectively.

Recognition and (semi-)quantitative analysis of REE-bearing minerals in coal using automated scanning electron microscopy

The recognition and quantification of rare earth and yttrium (REY) minerals in coal is extremely important for understanding their geological origin and developing high-efficiency extraction techniques. This study developed an automated image analysis by scanning electron microscopy (AIA-SEM) method for characterizing REY minerals in coal. Carbon and copper were used as grey-scale calibration standard to assure the consistency per experiment and differentiate organic matter and minerals with different brightness. Two critical issues in determining REY including rapid recognition of fine REY-bearing particles and accurate classification and quantification of REY minerals in coal are resolved by (1) establishing grey threshold standard to locate REY-bearing grains and a two-step image scan; (2) developing classification criteria supplemented with spot- and EDS-mapping analysis for questionable particles. By using the established method, a total of 166 REY-bearing mineral grains were identified from 12,930 particles in a medium-volatile bituminous coal (REY concentration: 149.21 ppm; ash yield: 21.25%). It is found that Ca-REE flurocarbonates, monazite, and (Sc, Y)-bearing zircon are the dominant REY species in the studied coal sample. REE-aluminophosphates are also important hosts for REE in coal, with total amounts being >10%. REY minerals are fine in particle size. Over 50% of monazite, xenotime, Ca-REE flurocarbonate, and REE-aluminophosphate have particle size below 5 μm and monazite occurs mostly as submicron particle. Most REY minerals (> 60%) are embedded into coal macerals as included minerals. About 80% of REY-bearing phosphates and zircon are partly or completely encapsulated in clay minerals, whereas more than half of Ca-REY-fluorocarbonates mineral grains is free of other minerals.

Relation of nonmetallic inclusions to the cyclic properties of steel 42CrMo4 after steel melt cleaning by filtration and related processes

Nonmetallic inclusions (NMIs) detrimentally influence the steel properties. The application of metal melt filter systems promises to reduce NMIs in steel. In the current work, NMIs are analyzed from metallographic sections after metal melt filtration or cleaning by a related process of the steel 42CrMo4 using immersion filtration, flow-through filtration as well as filters floating on top of the melt. Analyses by automated scanning electron microscopy (ASPEX) as well as light optical microcopy (LOM) revealed the chemistry, size distribution, and morphology of NMIs. The filter systems had a significant effect on these characteristics of NMIs. The threshold value ΔKth against fatigue crack propagation was found to depend on the amount of NMIs within the steel. A higher amount of NMIs caused less crack deflection leading to less roughness-induced crack closure and in turn resulted in lower threshold values at a stress ratio of R = 0.1. The comparison of the present analysis of NMIs with fatigue data from previous work indicated that the analysis of NMIs from metallographic sections can be used to approximate the fatigue strength of a batch in the same way as the analysis of NMIs from fatigue fracture surfaces for single specimens, as suggested by Murakami.

AI assisted steel cleanness evaluation: Predicting the morphology of La-traced non-metallic inclusions using backscattered-electron images

This study shows how computer vision, a field of artificial intelligence (AI), can be used to gain access to morphological information for a better process understanding and furthermore, how it can be implemented in the evaluation of active tracing experiments. Non-metallic inclusions (NMIs) play a crucial role in determining the chemical and physical properties of the final steel product. The active tracing technique allows for tracking the formation and modification mechanisms of detrimental NMIs throughout the steelmaking process by adding rare earth elements (REEs) to the melt. The interaction of REEs with NMIs results in the formation of traced multiphase particles and, therefore, lead to challenges for accurate evaluation by automated scanning electron microscopy with energy-dispersive spectroscopy (SEM/EDS). However, obtaining information about the REE distribution in traced NMIs without extensive, time-consuming human effort is not feasible using the existing method. A two-step classification process with AI was established, which included training and testing of two random forest classifiers (RFC). The first RFC achieved for the binary NMI/non-NMI classification an accuracy of 94.8 %. Four different morphology-based classes were considered in the second classification, whereas traced homogeneous NMIs and NMIs with a high La content got classified with a precision exceeding 90 %. However, caution is required in interpreting results for traced heterogeneous NMIs, as they have a higher prediction error of 37.2 %.

Novel technique for the preparation and analysis of powder-based polished sections by automated optical mineralogy: Part 2 – Use of deep learning approach for transparent mineral detection

Automated reflected light optical microscopy represents an alternative and affordable technique compared to automated scanning electron microscopy for quantitative mineralogical analysis. Polished sections are the commonly used sample analysis format, and it is essential to obtain unbiased mineralogical quantification results from those. However, automated optical microscopy does not allow the detection of transparent minerals during reflected light analysis, as the reflectivity of the resin and these minerals is very similar.This work aims to propose an innovative way to automatically detect all particles and minerals, including transparent minerals, in polished sections with acrylic resin using reflected light optical imaging and a deep learning algorithm. To do so, several ore powders and standard mineral mixes were mounted into acrylic resin polished sections at two different particle sizes: < 1 mm and P80 ∼ 75 µm. Optical images of these polished sections were acquired with an automated reflected light optical microscope to train and test the deep learning algorithm to detect mineral particles. The results suggest that the deep learning algorithm easily detected all mineral particles in the acrylic resin matrix, allowing all minerals particles (including transparent minerals) to be well-differentiated under reflected light optical microscopy, and providing an unbiased mineralogical quantification.

Hydrophilic cryogels as potential 3D cell culture materials: Synthesis and characterization of 2‐(methacrylamido) glucopyranose‐based polymer scaffolds

AbstractCell cultures are important techniques to investigate cellular processes in a simplified manner. The most commonly applied 2D models do not simulate most of the in vivo conditions whereas cryogels as promising 3D cell culture materials are able to provide both a structured microenvironment and tailored surface properties, similar to the natural extracellular matrix (ECM). Herein, we present the synthesis and characterization of hydrophilic cryogels with different 2‐(methacrylamido) glucopyranose amounts followed by 3D cell culture experiments with L929 cells. Selected samples are additionally functionalized with fibronectin‐FITC for improved cellular adhesion. The incorporation of different 2‐(methacrylamido) glucopyranose amounts into the cryogels is demonstrated by Fourier‐transform IR (FTIR) and solid‐state NMR (ssNMR). The gels are able to withstand harsh autoclaving conditions as shown by thermogravimetric analysis (TGA) and ssNMR measurements. Pore size measurements by automated scanning electron microscopy (SEM) image analysis reveal similar pore sizes among the entire cryogel series. Confocal laser scanning microscopy (CLSM) images suggest the presence of healthy cells due to the absence of morphological abnormalities among the entire cryogel series. L929 cells settled deeper into the cryogels with increasing MAG content. With additional fibronectin functionalization, the cells are retained much stronger and stay in the upper gel layers.

Formation and Modification of Al2O3 and MnS Inclusions in Al-Killed Gear Steels via Ca Treatment

A laboratory study was carried out to better understand the factors that contribute to the formation of complex inclusions, as inclusions play an important role during steel production; if not properly managed, inclusions can cause nozzle clogging during continuous casting and also damage the steel’s mechanical properties and machineability. To determine the chemical composition of inclusions that are less detrimental to the machineability of Al-deoxidized and Ca-treated gear steels, thermodynamic calculations and automated scanning electron microscopy (SEM) coupled with energy dispersive spectroscopy (EDS), as well as electron probe micro-X-ray analysis (EPMA) with the wavelength dispersive spectroscopy (WDS) technique, were utilized. The findings demonstrated that the morphology of inclusions changed from irregular to a more spherical type and the composition also changed to dual oxy-sulfides from pure oxides and sulfides as the Ca concentration in the steel was increased up to 36 ppm. The amount of Pure MnS sulfides also reduced significantly after Ca treatment. The ternary phase diagram and stability diagram for the inclusions revealed that 15–25 ppm Ca is the optimal range for the modification of both oxides and sulfides into the desired morphology and composition under the stipulation that the concentration of O in the steel is maintained at or below 50 ppm.

Analysis of Size Distribution, Chemical Composition, and Optical Properties of Mineral Dust Particles from Dry Deposition Measurement in Tenerife: Determined by Single-Particle Characterization

In this paper, individual particle analysis by automated scanning electron microscopy (SEM) coupled with energy-dispersive X-ray (EDX) was used to assess the size-resolved information of composition, size distribution, complex refractive index, and mixing state of mineral dust aerosol particles collected using different passive and active samplers. In the study, over 120,000 particles from 53 samples were analyzed. Results show that dust particles are the dominating mineral particle type during this campaign, comprising different classes of silicates, Si-rich (quartz-like), Ca-rich (calcite-like), CaMg-rich (dolomite-like), and CaS-rich (gypsum-like). The results also show that there is no significant difference in composition between suspended and deposited dust particles. By using the particle composition, the size-resolved complex refractive index of dust particles was calculated. The real part of the refractive index varied between 1.71 and 1.53 for wavelengths in the range of 370 to 950 nm. The imaginary part of the refractive index, determined mostly by iron oxide, varied between 3.28×10−4 and 7.11×10−5 for wavelengths ranging from 250 nm to 1640 nm. In addition, the refractive index values showed a slight decrease with increasing particle size. We also analyzed the potential for buffering of the acid mobilization of iron by other dust compounds. For particles which contain both iron (Fe) and (unprocessed) calcium (Ca), acids that are able to dissolve insoluble Fe particles can react with the Ca particles before reacting with Fe, but eventually, with longer processing time, the Fe particles could be processed. By analyzing the ratio of sulfate mass to the total aerosol mass of individual particles, the mixing state of sulfate particles to the total dust particles was investigated. The analysis showed that the finer dust particles were associated with higher content of sulfate, while the coarse dust particles correspond to lower sulfate contents, revealing that only fine mode sulfate is more internally mixed with mineral dust aerosol particles.

Digital biology approach for macroscale studies of biofilm growth and biocide effects with electron microscopy

Combination of automated scanning electron microscopy and a comprehensive software system that uses deep neural networks to perform an in-depth analysis of biofilms.

Quantitative analysis and formation mechanisms of non-metallic inclusions in GH4068 alloy prepared by vacuum induction melting

An automatic scanning electron microscope (SEM) analysis system and a self-designed superalloy inclusion analysis module were utilized to characterize the inclusions in the GH4068 Ni–Co-based superalloy prepared by vacuum induction melting (VIM). The morphologies, compositions, and distribution of the inclusions as well as the relationship between the contents of oxygen/nitrogen and inclusion were analyzed. The results indicate that the inclusions in the GH4068 alloy mainly include oxides, carbides, nitrides, carbonitrides and complex inclusions. The oxides are mainly concentrated in the top center of the cast ingots, and their content is higher than that at the bottom and edge. Nitrides and complex inclusions are mainly distributed near the bottom and edge of ingots. The analyses of thermodynamics indicate that the homogeneous nucleation of Al2O3 is spontaneous during the solidification although TiN prefers to wrap on the nucleated particles rather than homogeneously precipitate from the melt. The increase of oxygen/nitrogen content results in the increase of oxides, nitrides and complex inclusions. However, when the concentration of nitrogen is in the range of 3–12 ppm, the increase of nitrogen content shows negligible influence on the content of nitride inclusions.

Nanoindentation of alumina and multiphase inclusions in 42CrMo4 steel

Cleaning filter systems for metal melt filtration combine reactive filtration by functionalized filter surfaces for chemical reaction with the steel melt and active (mechanical) filtration. In the present work, a combined cleaning filter system was applied to 42CrMo4 steel melt containing nonmetallic inclusions, which were generated artificially before filtration. The nonmetallic inclusions in the solidified steel were investigated by an automated scanning electron microscope (ASPEX), nanoindentation, atomic force microscopy (AFM), focused ion beam technique (FIB) and confocal laser scanning microscopy (CLSM). The combined filter system was found to reduce the amount of aluminum in the steel and to form novel multiphase inclusions. These multiphase inclusions consist of TiO 2-x and Al 2 O 3 in a low-melting spessartine matrix and were characterized by nanoindentation. Compared to pure Al 2 O 3 inclusions, the spessartine inclusions are softer and have a lower Young's modulus, fitting much better to the mechanical properties of the steel. The area below the indents was investigated by focused ion beam technique and transmission scanning electron microscopy revealing cracks and dislocations. Furthermore, the low-melting character of the spessartine matrix was proven by means of a confocal laser scanning microscope. Accordingly, the low-melting spessartine inclusions appear as liquid inclusions during steel melt processing and could contribute to clogging prevention in continuous steel casting. • Combined steel melt filtration system caused formation of multiphase inclusions. • Multiphase inclusions entrapped TiO2-x and Al2O3 in a matrix of soft spessartine. • During nanoindentation of Al2O3, pop-in events marked elastic-plastic transition. • Analysis of EBSD data by MTEX suggest activation of pyramidal slip system in Al2O3. • Beneath the indents, plastic zone based on dislocations was observed by t-SEM.

Indicator mineral analyses of stream-sediment samples using automated mineralogy and mineral chemistry: Applicability to exploration in covered terranes in eastern Alaska, USA

In the past two decades, significant research efforts have been devoted to porphyry copper indicator mineral (PCIM) identification and mineral chemistry to assist exploration. Such studies are important in the Yukon-Tanana upland region of eastern Alaska because well-established geochemical exploration techniques, such as the geochemistry of stream-sediment samples, are less effective in the search for mineral resources owing to cover materials that subdue geochemical signatures. The unglaciated Yukon-Tanana upland region is well-endowed with mineral resources, including porphyry Cu-Mo-Au deposits at Taurus, Bluff, Dennison, and Oreo. Using automated scanning electron microscope (SEM) techniques, numerous PCIMs have been identified in rocks and stream-sediment samples that would likely not have been observed using visual binocular microscope methods. Sulfide minerals such as chalcopyrite, chalcocite, covellite, bornite, molybdenite, and pyrrhotite were identified in rock samples, and more than half of the stream-sediment samples from drainages containing known porphyry mineral occurrences contain chalcopyrite with or without bornite. Many drainages without known occurrences also contain these minerals, which suggests potential for additional occurrences. Svanbergite, an aluminum phosphate sulfate (APS) mineral [SrAl3(PO4)(SO4)(OH)6], was identified in some of the altered or mineralized rock samples from Taurus, and in stream drainages containing porphyry occurrences and may represent the best indicator mineral for Taurus-like porphyry deposits. Apatite chemistry has great potential as a tool for assessing the presence of porphyry mineralization. Grains from rock and stream-sediment samples that contain high Cl (>∼0.4 wt%), Fe (>0.4 wt%), and Mn (>2000 ppm) clearly distinguish apatite from other sources (metamorphic, unmineralized igneous rocks). This study is one of the first to document new streamlined indicator mineral sample collection and processing methods and to combine automated SEM techniques and chemistry of minerals derived from both bedrock and surficial (stream) sediments as they apply to porphyry exploration.

Mineralogical and microtextural characterization of eco-friendly concrete for marine infrastructures: Methodologies for the MARINEFF Project

The European cross-border Project MARINEFF explores the use of eco-friendly concrete materials in the construction of marine structures (oyster bed modules, dykes, boat moorings and rockpools). The structures and materials are designed to protect and improve the local biodiversity of the marine environment of the Channel / La Manche. This paper focuses on the mineralogical and microtextural characterization of the concrete materials. The aim is to introduce how advanced analytical methods have been employed to gain an understanding of the evolution of the materials, in particular their response to immersion into the sea. Our methods include the traditional techniques for examining concrete materials (optical microscopy, scanning electron microscopy, X-ray diffraction), but also introduces the benefits of mineralogical methods that go beyond the current “state-of-the-art” (automated scanning electron microscopy by QEMSCAN®, electron-probe microanalysis). Our results offer detailed insight into the controls on the compositional and structural evolution of the materials.

Modification Mechanism of Lanthanum on Alumina Inclusions in a Nonoriented Electrical Steel

The modification mechanism of lanthanum on alumina inclusions in a nonoriented electrical steel at 1600 °C is investigated using laboratory experiments. Inclusions are analyzed using an automatic scanning electron microscope equipped with energy‐dispersive spectrum at 1, 5, 10, and 30 min after lanthanum treatment. The contents of total oxygen (TO), total sulfur (TS), and total lanthanum (TLa) in steel are analyzed. Results show that Al2O3 inclusions are modified by lanthanum in two ways. One is that the dissolved lanthanum directly reduces the aluminum in Al2O3 inclusions and forms LaAl11O18 or LaAlO3 ones. The other is that a new La2O2S or LaS x shell is preferentially generated at the outside of Al2O3 and forms multiphase inclusions. With time increasing, the La2O2S or LaS x shell gradually reacts with the Al2O3 core and generates stable lanthanum‐containing inclusions. At the initial stage of lanthanum treatment, many transient inclusions including LaS x , La2O2S, and La–P(–As) are formed due to the high concentration of lanthanum, while gradually redissolving with time increasing. With the increase in TLa content in steel, the formation sequence of stable inclusions is Al2O3 → LaAl11O18 → LaAlO3 → La2O2S → LaS x , which is consistent with thermodynamic analysis.

Effect of Rare Earth Cerium Content on Manganese Sulfide in U75V Heavy Rail Steel

To study the effect of Ce on the morphology of manganese sulfide, we added different contents of Ce into U75V heavy rail steel. The composition and morphology of sulfide in steel were analyzed. The inclusions’ number, size, and aspect ratio were analyzed by automatic scanning electron microscope ASPEX. The results show that the inclusions in heavy rail steel without Ce are elongated MnS and irregular Al-Si-Ca-O inclusions. With the increase of Ce from 52 ppm to 340 ppm, the composition of main inclusions changes along the route of Ce2O2S-MnS → Ce2O2S-MnS-Ce2S3 → Ce2O2S-Ce3S4-Ce2S3 → Ce2O2S-Ce3S4-CeS. Ce has a noticeable spheroidization effect on MnS, which can make inclusions finely dispersed. When Ce content is 139 ppm, the average size of inclusions is the smallest. The mechanism of Ce-modified MnS was discussed by combining experimental results with thermodynamic calculations. Finally, the effect of Ce treatment on inhibiting MnS deformation was verified by simulated rolling.

The sampling and phase characterisation of black mass

“Black mass” is the industry term used to describe a type of e-waste comprising crushed and shredded battery cells. It is an intermediate product in the recycling of spent, end-of-life, batteries. It comprises a mixture of metals including; lithium, manganese, cobalt and nickel, which are valuable recycling commodities, of increasing strategic and economic importance to meet future global demands in the “battery revolution”. The objective of this “phase characterisation” investigation was to provide an indicative profile of the morphological characteristics, grain size, composition and textural variability for a natural state (unprepared) and prepared (powdered) sample of black mass from Europe. It is envisaged that this is relevant to: (a) develop a pragmatic sampling strategy to ensure a non-biased, representative sample is provided for assaying; (b) determine the optimal processing route (e.g., hydrometallurgical, pyrometallurgical); (c) identify the presence of payable phases; (d) identify phases that may hinder metal recovery or penalty components; (e) develop assay procedures; and (f) assist in the identification of hazards and the mitigation of risks. The techniques used were: (1) visual examination and binocular microscopy; (2) manual scanning electron microscopy (SEM); (3) automated scanning electron microscopy with linked energy dispersive spectrometers (SEM-EDS), to characterise the phases present and particle types (using AMICS); (4) X-ray computed tomography (X-CT) to provide the 3D morphology of the particles; and (5) laser ablation inductively-coupled plasma mass spectrometry (LA-ICP-MS) to detect and quantify the phases that cannot be detected using automated SEM-EDS and X-CT. The results demonstrated that automated SEM-EDS can be used to characterise and quantify the phases present, and the phase chemistry allows the particle types to be assigned back to the primary battery components. Some phases identified are at present not linked back to the original components and further work is needed to refine the compositional groups, with the analysis of additional samples from different feeds/streams in Europe, China and USA. Interactive SEM-EDS analysis also demonstrated that there is a high-resolution chemical variability within the individual particle categories. X-CT imaging demonstrated the complex 3D textures and morphology of the particles, which is potentially significant during sample preparation and chemical analysis. Neither automated nor manual interactive analysis can determine the presence / abundance of the light elements, such as lithium. However, LA-ICP-MS was successful in detecting and quantifying lithium. Furthermore, LA-ICP-MS was able to determine contents of 67 other non-metals and metals at a 20-micron scale with ppm to ppb level detection limits.

Influence of Nickel on Niobium Nitride Formation in As-Cast Stainless Steels

The influence of the nickel content and cooling rate on niobium nitride precipitation in as-cast stainless steels were analysed. Niobium microalloying is important for mechanical properties and the prevention of intergranular corrosion in stainless steels. However, coarse precipitates can negatively affect steel properties. The precipitation of NbN depends on thermodynamic conditions, which are dictated by the chemical composition and temperature. The thermodynamic computations were used to estimate niobium nitride precipitation. Additionally, segregation models were used to predict precipitation. Three steel batches with different nickel contents (9 wt.%, 4.7 wt.%, and 0.16 wt.%) were prepared in an induction furnace and cast into sand moulds. The polished and etched samples were examined with an optical microscope, followed by a more detailed examination using a scanning electron microscope. An automatic scanning electron microscope analysis of the niobium particles was performed to obtain particle number and size distribution. Primary niobium carbonitrides, eutectic phases, and heterogenous nucleations on MnS inclusions were observed. As the proportion of nickel in the solution decreased, the solubility of nitrogen in the melt increased, which is manifested by a lower formation of primary and eutectic niobium carbonitrides, while MnS non-metallic inclusions played an important role in the heterogeneous nucleation.