scholarly journals Speciation of Manganese in a Synthetic Recycling Slag Relevant for Lithium Recycling from Lithium-Ion Batteries

Metals ◽  
2021 ◽  
Vol 11 (2) ◽  
pp. 188
Author(s):  
Alena Wittkowski ◽  
Thomas Schirmer ◽  
Hao Qiu ◽  
Daniel Goldmann ◽  
Ursula E. A. Fittschen
Keyword(s):  
Solid Solution ◽  
Inductively Coupled Plasma ◽  
Lithium Ion ◽  
Manganese Concentration ◽  
Aluminum Concentration ◽  
Emission Spectrometry ◽  
Lithium Aluminum ◽  
Spinel Solid Solution ◽  
Edge Structure ◽  
X Ray

Lithium aluminum oxide has previously been identified to be a suitable compound to recover lithium (Li) from Li-ion battery recycling slags. Its formation is hampered in the presence of high concentrations of manganese (9 wt.% MnO2). In this study, mock-up slags of the system Li2O-CaO-SiO2-Al2O3-MgO-MnOx with up to 17 mol% MnO2-content were prepared. The manganese (Mn)-bearing phases were characterized with inductively coupled plasma optical emission spectrometry (ICP-OES), X-ray diffraction (XRD), electron probe microanalysis (EPMA), and X-ray absorption near edge structure analysis (XANES). The XRD results confirm the decrease of LiAlO2 phases from Mn-poor slags (7 mol% MnO2) to Mn-rich slags (17 mol% MnO2). The Mn-rich grains are predominantly present as idiomorphic and relatively large (>50 µm) crystals. XRD, EPMA and XANES suggest that manganese is present in the form of a spinel solid solution. The absence of light elements besides Li and O allowed to estimate the Li content in the Mn-rich grain, and to determine a generic stoichiometry of the spinel solid solution, i.e., (Li(2x)Mn2+(1−x))1+x(Al(2−z),Mn3+z)O4. The coefficients x and z were determined at several locations of the grain. It is shown that the aluminum concentration decreases, while the manganese concentration increases from the start (x: 0.27; z: 0.54) to the end (x: 0.34; z: 1.55) of the crystallization.

scholarly journals Classification of spent Li-ion batteries based on ICP-OES/X-ray characterization of the cathode materials

2020 ◽  
Vol 74 (3) ◽  
pp. 221-230
Author(s):  
Dragana Medic ◽  
Snezana Milic ◽  
Sladjana Alagic ◽  
Ivan Djordjevic ◽  
Silvana Dimitrijevic
Keyword(s):  
Chemical Composition ◽  
Cathode Material ◽  
Cathode Materials ◽  
Inductively Coupled Plasma ◽  
Lithium Ion ◽  
Rapid Expansion ◽  
Emission Spectrometry ◽  
X Ray ◽  
Spent Libs

Development of lithium-ion batteries (LIBs) during the latest decades resulted in improved performances of the new integrated cathode materials and in their wide applications. This rapid expansion of new materials led to the intensive replacement of the old-fashioned, traditional materials and increased a simultaneous accumulation of both kinds of materials at extremely hazardous electronic waste sites, which additionally increased an urgent need for their recycling. Most importantly, in this way, spent LIBs may further serve as a significant source of valuable metals such as Li and cobalt. However, one of the key problems in LIBs recycling is the absence of a precise battery classification/sorting based on the chemical composition of the used cathode material. In this paper, characterization of the cathode material was performed regarding chemical composition of 40 samples of spent LIBs using inductively coupled plasma - optical emission spectrometry and X-ray diffraction. Preparation of the samples, (pretreatment) included: discharging, dismantling, separation of the main components (cathode, anode and the separator), and detachment of the cathode material from the aluminium foil. The obtained results showed that, in the investigated commercially available LIBs, lithium cobalt oxide was the most frequently used (cathode) material.

scholarly journals INCORPORATION OF Mo6+ IN FERRIHYDRITE, GOETHITE, AND HEMATITE

2021 ◽  
Author(s):  
Marcel G. Görn ◽  
Ralph M. Bolanz ◽  
Stephen Parry ◽  
Jörg Göttlicher ◽  
Ralph Steininger ◽  
...  
Keyword(s):  
Inductively Coupled Plasma ◽  
Structural Disorder ◽  
Unit Cell ◽  
Emission Spectrometry ◽  
Charge Balance ◽  
Unit Cell Parameters ◽  
Edge Structure ◽  
X Ray ◽  
Cell Parameters ◽  
X Ray Absorption

AbstractAmong all iron oxides, hematite (α-Fe2O3), goethite (α-FeOOH), and ferrihydrite (FeOOH⋅nH2O) are the most common mineral species. While immobilization of Mo6+ by surface adsorption on ferric oxides has been studied extensively, the mechanisms of incorporation in their structure have been researched little. The objective of this study was to investigate the relation between Mo content and its structural incorporation in hematite, goethite, and six-line ferrihydrite by a combination of X-ray absorption spectroscopy (XAS), powder X-ray diffraction (pXRD), and inductively-coupled plasma optical emission spectrometry (ICP-OES). Synthesized in the presence of Mo, the hematite, goethite, and six-line ferrihydrite phases incorporated up to 8.52, 0.03, and 17.49 wt. % Mo, respectively. For hematite and goethite, pXRD analyses did not indicate the presence of separate Mo phases. Refined unit-cell parameters correlated with increasing Mo concentration in hematite and goethite. The unit-cell parameters indicated an increase in structural disorder within both phases and, therefore, supported the structural incorporation of Mo in hematite and goethite. Analysis of pXRD measurements of Mo-bearing six-line ferrihydrites revealed small amounts of coprecipitated akaganéite. X-ray absorption near edge structure (XANES) measurements at the Mo L3-edge indicated a strong distortion of the MoO6 octahedra in all three phases. Fitting of extended X-ray absorption fine structure (EXAFS) spectra of the Mo K-edge supported the presence of such distorted octahedra in a coordination environment similar to the Fe position in the investigated specimen. Incorporation of Mo6+ at the Fe3+-position for both hematite and goethite resulted in the formation of one Fe vacancy in close proximity to the newly incorporated Mo6+ and, therefore, charge balance within the hematite and goethite structures.

scholarly journals Distribution and Mode of Occurrence of Co, Ni, Cu, Zn, As, Ag, Cd, Sb, Pb in the Feed Coal, Fly Ash, Slag, in the Topsoil and in the Roots of Trees and Undergrowth Downwind of Three Power Stations in Poland

Minerals ◽  
2021 ◽  
Vol 11 (2) ◽  
pp. 133
Author(s):  
Henryk R. Parzentny ◽  
Leokadia Róg
Keyword(s):  
Inductively Coupled Plasma ◽  
Coal Fly Ash ◽  
Atomic Emission ◽  
Emission Spectrometry ◽  
Plasma Atomic Emission Spectrometry ◽  
X Ray ◽  
Inductively Coupled ◽  
Power Stations ◽  
Mode Of Occurrence ◽  
Feed Coal

It is supposed that the determination of the content and the mode of occurrence of ecotoxic elements (EE) in feed coal play the most significant role in forecasting distribution of EE in the soil and plants in the vicinity of power stations. Hence, the aim of the work was to analyze the properties of the feed coal, the combustion residues, and the topsoil which are reached by EE together with dust from power stations. The mineral and organic phases, which are the main hosts of EE, were identified by microscopy, X-ray powder diffraction, inductively coupled plasma atomic emission spectrometry, and scanning electron microscope with an energy dispersive X-ray methods. The highest content of elements was observed in the Oi and Oe subhorizons of the topsoil. Their hosts are various types of microspheres and char, emitted by power stations. In the areas of long-term industrial activity, there are also sharp-edged grains of magnetite emitted in the past by zinc, lead, and ironworks. The enrichment of the topsoil with these elements resulted in the increase in the content of EE, by between 0.2 times for Co; and 41.0 times for Cd in the roots of Scots pine, common oak and undergrowth, especially in the rhizodermis and the primary cortex and, more seldom, in the axle roller and cortex cells.

scholarly journals The Effect of Mg and Zn Dopants on Pt/Al2O3 for the Dehydrogenation of Perhydrodibenzyltoluene

Catalysts ◽  
2021 ◽  
Vol 11 (4) ◽  
pp. 490
Author(s):  
Rudaviro Garidzirai ◽  
Phillimon Modisha ◽  
Innocent Shuro ◽  
Jacobus Visagie ◽  
Pieter van Helden ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Inductively Coupled Plasma ◽  
Flow Reactor ◽  
Plug Flow ◽  
Optical Emission ◽  
Catalytic Performance ◽  
Emission Spectrometry ◽  
Hydrogen Yield ◽  
X Ray ◽  
Temperature Programmed

The effects of Mg and Zn dopants on the catalytic performance of Pt/Al2O3 catalyst were investigated for dehydrogenation of perhydrodibenzyltoluene (H18-DBT) as a liquid organic hydrogen carrier. Al2O3 supports were modified with Mg and Zn to produce Mg-Al2O3 and Zn-Al2O3 with a target loading of 3.8 wt.% for dopants. The modified supports were impregnated with chloroplatinic acid solution to produce the catalysts Pt/Al2O3, Pt/Mg-Al2O3 and Pt/Zn-Al2O3 of 0.5 wt.% Pt loading. Thereafter, the catalysts were characterised using inductively coupled plasma- optical emission spectrometry, scanning electron microscopy-energy dispersive X-ray spectroscopy, hydrogen temperature-programmed reduction, carbon-monoxide pulse chemisorption, ammonia temperature-programmed desorption, X-ray diffraction and transmission electron microscopy. The dehydrogenation experiments were performed using a horizontal plug flow reactor system and the catalyst time-on-stream was 22 h. Pt/Mg-Al2O3 showed the highest average hydrogen flowrate of 29 nL/h, while an average of 27 nL/h was obtained for both Pt/Al2O3 and Pt/Zn-Al2O3. This has resulted in a hydrogen yield of 80% for Pt/Mg-Al2O3, 71% for Pt/Zn-Al2O3 and 73% for Pt/Al2O3. In addition, the conversion of H18-DBT ranges from 99% to 92%, Pt 97–90% and 96–90% for Pt/Mg-Al2O3, Pt/Zn-Al2O3 and Pt/Al2O3, respectively. Following the latter catalyst order, the selectivity to dibenzyltoluene (H0-DBT) ranges from 78% to 57%, 75–51% and 71–45%. Therefore, Pt/Mg-Al2O3 showed improved catalytic performance towards dehydrogenation of H18-DBT.

scholarly journals The effect of cobalt on morphology, structure, and ORR activity of electrospun carbon fibre mats in aqueous alkaline environments

2021 ◽  
Vol 12 ◽  
pp. 1173-1186
Author(s):  
Markus Gehring ◽  
Tobias Kutsch ◽  
Osmane Camara ◽  
Alexandre Merlen ◽  
Hermann Tempel ◽  
...  
Keyword(s):  
Photoelectron Spectroscopy ◽  
Inductively Coupled Plasma ◽  
Elevated Temperatures ◽  
Current Collector ◽  
Alkaline Media ◽  
Emission Spectrometry ◽  
Free Standing ◽  
X Ray ◽  
Turbostratic Carbon ◽  
Current Densities

An innovative approach for the design of air electrodes for metal–air batteries are free-standing scaffolds made of electrospun polyacrylonitrile fibres. In this study, cobalt-decorated fibres are prepared, and the influence of carbonisation temperature on the resulting particle decoration, as well as on fibre structure and morphology is discussed. Scanning electron microscopy, Raman spectroscopy, X-ray diffraction, X-ray photoelectron spectroscopy, elemental analysis, and inductively coupled plasma optical emission spectrometry are used for characterisation. The modified fibre system is compared to a benchmark system without cobalt additives. Cobalt is known to catalyse the formation of graphite in carbonaceous materials at elevated temperatures. As a result of cobalt migration in the material the resulting overall morphology is that of turbostratic carbon. Nitrogen removal and nitrogen-type distribution are enhanced by the cobalt additives. At lower carbonisation temperatures cobalt is distributed over the surface of the fibres, whereas at high carbonisation temperatures it forms particles with diameters up to 300 nm. Free-standing, current-collector-free electrodes assembled from carbonised cobalt-decorated fibre mats display promising performance for the oxygen reduction reaction in aqueous alkaline media. High current densities at an overpotential of 100 mV and low overpotentials at current densities of 333 μA·cm−2 were found for all electrodes made from cobalt-decorated fibre mats carbonised at temperatures between 800 and 1000 °C.

Early commissioning results for spectroscopic X-ray Nano-Imaging Beamline BL 7C sXNI at PLS-II

2017 ◽  
Vol 24 (6) ◽  
pp. 1276-1282 ◽  
Author(s):  
Sangsul Lee ◽  
Ik hwan Kwon ◽  
Jae-Young Kim ◽  
Sung-Sun Yang ◽  
Sechang Kang ◽  
...  
Keyword(s):  
Lithium Iron Phosphate ◽  
Phase Distribution ◽  
Lithium Ion ◽  
Feedback System ◽  
Double Crystal ◽  
Pilot Studies ◽  
Beam Position ◽  
Edge Structure ◽  
X Ray

For spectral imaging of chemical distributions using X-ray absorption near-edge structure (XANES) spectra, a modified double-crystal monochromator, a focusing plane mirrors system and a newly developed fluorescence-type X-ray beam-position monitoring and feedback system have been implemented. This major hardware upgrade provides a sufficiently stable X-ray source during energy scanning of more than hundreds of eV for acquisition of reliable XANES spectra in two-dimensional and three-dimensional images. In recent pilot studies discussed in this paper, heavy-metal uptake by plant rootsin vivoand iron's phase distribution in the lithium–iron–phosphate cathode of a lithium-ion battery have been imaged. Also, the spatial resolution of computed tomography has been improved from 70 nm to 55 nm by means of run-out correction and application of a reconstruction algorithm.

scholarly journals Geological Controls on Mineralogy and Geochemistry of the Permian and Jurassic Coals in the Shanbei Coalfield, Shaanxi Province, North China

Minerals ◽  
2020 ◽  
Vol 10 (2) ◽  
pp. 138
Author(s):  
Yunfei Shangguan ◽  
Xinguo Zhuang ◽  
Jing Li ◽  
Baoqing Li ◽  
Xavier Querol ◽  
...  
Keyword(s):  
Inductively Coupled Plasma ◽  
North China ◽  
Ordos Basin ◽  
Source Region ◽  
Atomic Emission ◽  
Shaanxi Province ◽  
Emission Spectrometry ◽  
Plasma Atomic Emission Spectrometry ◽  
X Ray ◽  
Diagenetic Fluid

Coal as the source of critical elements has attracted much attention and the enrichment mechanisms are of significant importance. This paper has an opportunity to investigate the mineralogical and geochemical characteristics of the Permian and Jurassic bituminous coals and associated non-coals from two underground coal mines in the Shanbei Coalfield (Northeast Ordos basin), Shaanxi Province, North China, based on the analysis of X-ray diffraction (XRD), inductively coupled plasma atomic-emission spectrometry (ICP-AES/MS), and scanning electron microscopy-energy-dispersive X-ray spectroscopy (SEM-EDS). The Jurassic and Permian coals have similar chemical features excluding ash yield, which is significantly higher in the Permian coals. Major mineral matters in the Jurassic coals are quartz, kaolinite, and calcite. By contrast, mineral assemblages of the Permian coals are dominated by kaolinite; and apatite occurring in the middle section’s partings. The Jurassic coals are only enriched in B, whereas the Permian coals are enriched in some trace elements (e.g., Nb, Ta, Th, and REY). Boron has a mixed inorganic and organic association which may be absorbed by organic matter from fluid (or groundwater) or inherited from coal-forming plants. Additionally, climatic variation also plays an important role. As for the Permian coals, kaolinite and apatite as the major carriers of elevated elements; the former were derived from the sedimentary source region (the Yinshan Oldland and the Benxi formation) and later precipitated from Ca-, and P-rich solutions. We deduced that those elevated elements may be controlled by the source rock and diagenetic fluid input. The findings of this work offered new data to figure out the mechanism of trace element enrichment of coal in the Ordos basin.

scholarly journals Oil-based mud waste reclamation and utilisation in low-density polyethylene composites

2020 ◽  
Vol 38 (12) ◽  
pp. 1331-1344
Author(s):  
Shohel Siddique ◽  
Kyari Yates ◽  
Kerr Matthews ◽  
Laszlo J Csetenyi ◽  
James Njuguna
Keyword(s):  
Inductively Coupled Plasma ◽  
Oil And Gas ◽  
Microscopic Analysis ◽  
Optical Emission ◽  
Fluorescence Analysis ◽  
Xrd Analysis ◽  
Low Density Polyethylene ◽  
Emission Spectrometry ◽  
Low Density ◽  
X Ray

Oil-based mud (OBM) waste from the oil and gas exploration industry can be valorised to tailor-made reclaimed clay-reinforced low-density polyethylene (LDPE) nanocomposites. This study aims to fill the information gap in the literature and to provide opportunities to explore the effective recovery and recycling techniques of the resources present in the OBM waste stream. Elemental analysis using inductively coupled plasma–optical emission spectrometry (ICP-OES) and X-ray fluorescence analysis, chemical structural analysis by Fourier transform infrared (FTIR) spectroscopy, and morphological analysis of LDPE/organo-modified montmorillonite (LDPE/MMT) and LDPE/OBM slurry nanocomposites by scanning electron microscopy (SEM) have been conducted. Further analysis including calorimetry, thermogravimetry, spectroscopy, microscopy, energy dispersive X-ray analysis and X-ray diffraction (XRD) was carried out to evaluate the thermo-chemical characteristics of OBM waste and OBM clay-reinforced LDPE nanocomposites, confirming the presence of different clay minerals including inorganic salts in OBM slurry powder. The microscopic analysis revealed that the distance between polymer matrix and OBM slurry filler is less than that of MMT, which suggests better interfacial adhesion of OBM slurry compared with the adhesion between MMT and LDPE matrix. This was also confirmed by XRD analysis, which showed the superior delamination structure OBM slurry compared with the structure of MMT. There is a trend noticeable for both of these fillers that the nanocomposites with higher percentage filler contents (7.5 and 10.0 wt% in this case) were indicated to act as a thermal conductive material. The heat capacity values of nanocomposites decreased about 33% in LDPE with 7.5 wt% MMT and about 17% in LDPE with 10.0 wt% OBM slurry. It was also noted, for both nanocomposites, that the residue remaining after 1000°C increases with the incremental wt% of fillers in the nanocomposites. There is a big difference in residue amount (in %) left after thermogravimetric analysis in the two nanocomposites, indicating that OBM slurry may have significant influence in decomposing LDPE matrix; this might be an interesting area to explore in the future. The results provide insight and opportunity to manufacture waste-derived renewable nanocomposites with enhanced structural and thermal properties.

scholarly journals Bulk Synthesis and Characterization of Ti3Al Nanoparticles by Flow-Levitation Method

2013 ◽  
Vol 2013 ◽  
pp. 1-5 ◽  
Author(s):  
Shanjun Chen ◽  
Yan Chen ◽  
Huafeng Zhang ◽  
Yongjian Tang ◽  
Jianjun Wei ◽  
...  
Keyword(s):  
Inductively Coupled Plasma ◽  
Synthesis Method ◽  
Atomic Emission ◽  
Hexagonal Structure ◽  
Emission Spectrometry ◽  
Plasma Atomic Emission Spectrometry ◽  
X Ray ◽  
Inductively Coupled ◽  
Al Nanoparticles ◽  
Ar Gas

A novel bulk synthesis method for preparing high pure Ti3Al nanoparticles was developed by flow-levitation method (FL). The Ti and Al vapours ascending from the high temperature levitated droplet were condensed by cryogenic Ar gas under atmospheric pressure. The morphology, crystalline structure, and chemical composition of Ti3Al nanoparticles were, respectively, investigated by transmission electron microscopy, X-ray diffraction, and inductively coupled plasma atomic emission spectrometry. The results indicated that the Ti3Al powders are nearly spherical-shaped, and the particle size ranges from several nanometers to 100 nm in diameter. Measurements of the d-spacing from X-ray (XRD) and electron diffraction studies confirmed that the Ti3Al nanoparticles have a hexagonal structure. A thin oxidation coating of 2-3 nm in thickness was formed around the particles after exposure to air. Based on the XPS measurements, the surface coating of the Ti3Al nanoparticles is a mixture of Al2O3and TiO2. The production rate of Ti3Al nanoparticles was estimated to be about 3 g/h. This method has a great potential in mass production of Ti3Al nanoparticles.

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