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At least 739 records · Page 41

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DOE OSTI2017

Dephosphorization Kinetics between Bloated Metal Droplets and Slag Containing FeO: The Influence of CO Bubbles on the Mass Transfer of Phosphorus in the Metal

Dephosphorization kinetics of bloated metal droplets was investigated in the temperature range from 1813 K to 1913 K (1540 °C to 1640 °C). The experimental results showed that the overall mass transfer coefficient, k{sub o}, decreased with increasing temperature because of decreasing phosphorus partition ratio, L P . It was also found that the mass transfer coefficient for phosphorus in the metal, k m , had the highest value at the lowest temperature [i.e., 1813 K (1540 °C)] because the formation of smaller CO bubbles increased the rate of surface renewal, leading to faster mass transport. Meanwhile, metal droplets without carbon were also employed to study the effect of decarburization on dephosphorization. The results show that although decarburization lowers the driving force significantly, k{sub m} (6.2 × 10 -2 cm/s) for a carbon containing droplet is two orders of magnitude higher than that for carbon free droplets (5.3 × 10 -4 cm/s) because of the stirring effect provided by CO bubbles. This stirring offers a faster surface renewal rate, which surpasses the loss of driving force and then leads to a faster dephosphorization rate.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Study on the Impact Characteristics of Coherent Supersonic Jet and Conventional Supersonic Jet in EAF Steelmaking Process

Supersonic oxygen-supplying technologies, including the coherent supersonic jet and the conventional supersonic jet, are now widely applied in electric arc furnace steelmaking processes to increase the bath stirring, reaction rates, and energy efficiency. However, there has been limited research on the impact characteristics of the two supersonic jets. In the present study, by integrating theoretical modeling and numerical simulations, a hybrid model was developed and modified to calculate the penetration depth and impact zone volume of the coherent and conventional supersonic jets. The computational fluid dynamics results were validated against water model experiments. The results show that the lance height has significant influence on the jet penetration depth and jet impact zone volume. The penetration depth decreases with increasing lance height, whereas the jet impact zone volume initially increases and then decreases with increasing lance height. In addition, the penetration depth and impact zone volume of the coherent supersonic jet are larger than those of the conventional supersonic jet at the same lance height, which illustrates the advantages of the coherent supersonic jet in delivering great amounts of oxygen to liquid melt with a better stirring effect compared to the conventional supersonic jet. A newly defined parameter, the k value, reflects the velocity attenuation and the potential core length of the main supersonic jet. Finally, a hybrid model and its modifications can well predict the penetration depth and impact zone volume of the coherent and conventional supersonic jets.

36 MATERIALS SCIENCE↗

DOE OSTI2017

Experimental Study on the Activities of Al and Ca in Ferrosilicon

Experiments were carried out to determine the activities of Al and Ca in liquid ferrosilicon (with about 50 wt pct Si) at 1823 K (1550 °C) in their dilution ranges. Liquid FeSi50 and SiO{sub 2}-Al{sub 2}O{sub 3}-CaO slag were stirred mechanically in a graphite crucible to enhance the transfer of Al and Ca between the two phases. The stirring time for the two phases to reach equilibrium was studied. It was found that a time of 45 minutes was long enough to reach the slag–metal equilibrium. The activities of Al and Ca in the ferrosilicon alloy were calculated based on the compositions of the two liquid phases. The activity coefficients obtained for Al and Ca in the liquid FeSi50 at 1823 K (1550 °C) were found to be nearly constant in the composition range studied.

36 MATERIALS SCIENCE↗

DOE OSTI2019

A Kinetic Model for Dissolution of Zinc Oxide Powder Obtained from Waste Alkaline Batteries in Sodium Hydroxide Solutions

The determination of individual dissolution behaviors of zinc and manganese in waste alkaline battery powders is an important subject from the points of the leaching yield, design of leaching reactor, and separation and recovery steps of hydrometallurgical process. In the current study, we investigated the dissolution kinetics of zinc oxide powder. Zinc oxide was obtained from waste alkaline batteries, and sodium hydroxide solutions were used as solvent. In the experiments, the effects of solution concentration, reaction temperature, stirring speed, solid-to-liquid ratio, and particle size on the dissolution of zinc oxide were investigated. It was demonstrated that the dissolution increased with the increasing concentration, reaction temperature, and stirring speed, and with the decreasing solid-to-liquid ratio and particle size. In consequence of the kinetic analysis performed, it was found that the dissolution kinetics of zinc powder obeyed the Avrami model. Activation energy for the process was determined to be 19.42 kJ/mol. Zinc ions in the resulting solution after dissolution process was recovered in the form of hydroxy-carbonate product by precipitation method. Zinc oxide was produced by isothermal decomposition of hydroxy-carbonate product.

36 MATERIALS SCIENCE↗

DOE OSTI2019

Recovery of Carbon and Valuable Components from Spent Pot Lining by Leaching with Acidic Aluminum Anodizing Wastewaters

A three-step process was employed to separate cryolite from used carbon cathodes, known as spent pot lining (SPL), and obtain valuable carbon. The process comprised leaching of NaF from the imbedded electrolyte with water, followed by leaching of Na{sub 3}AlF{sub 6}, CaF{sub 2}, and NaAl{sub 11}O{sub 17} with acidic anodizing wastewater, and then precipitating the electrolyte components from the mixed filtrate from the previous two steps. The influences of stirring rate, liquid–solid ratio, temperature, and time on the extent of leaching of cryolite and recovery of carbon were studied. Additionally, the effects of pH value, F/Al ratio, temperature, and time on the recovery of valuable components in the mixed filtrate were evaluated. The results showed that most NaF in the SPL was dissolved by water leaching. The residual electrolyte in SPL was mainly cryolite and contained approximately 0.95 pct NaF. The purity of the carbon obtained reached 95.5 pct under optimal experimental conditions (leaching temperature: 80 °C; stirring rate: 300 rpm; liquid–solid ratio: 8 mL/g; leaching time: 180 minutes). The recovery of cryolite and the purity of the sodium sulfate crystal from the mixed filtrate were 98.4 and 92.0 pct, respectively, under suitable conditions (pH 9; 75 °C; 4 hour; F/Al ratio of 6:1).

36 MATERIALS SCIENCE↗

DOE OSTI2019

Fluid Flow, Thermal Stratification, and Inclusion Motion During Holding Period in Steel Ladles

In the current study, the fluid flow and thermal stratification during the holding period are numerically simulated. The standard k–ε two-equation turbulence model is adopted to describe the turbulence. The trajectories of inclusions are calculated by the discrete phase model (DPM) considering the stochastic effect of turbulence. Two different initial conditions for the flow field are compared: the quiescent state of flow and the fluid flow induced by gas stirring. Significant differences are observed between these cases. In practice, the holding period starts from the shut-off of the gas blowing. Thus, it is proposed that the flow field at the terminal of gas stirring should be considered for the simulation of the fluid flow, heat transfer, and inclusion motion during the holding period.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Development of Graphene Nanoplatelet-Reinforced AZ91 Magnesium Alloy by Solidification Processing

It is a challenging task to effectively incorporate graphene nanoplatelets (GNPs) which have recently emerged as potential reinforcement for strengthening metals into magnesium-based matrices by conventional solidification processes due to their large surface areas and poor wettability. A solidification processing which combines mechanical stirring and ultrasonic dispersion of reinforcements in liquid matrix was employed to develop AZ91 magnesium alloy matrix composites reinforced with 0.25 and 0.5 wt.% GNPs. The microstructural studies conducted with scanning and transmission electron microscopes revealed that fairly uniform distribution and dispersion of GNPs through the matrix were achieved due to effective combination of mechanical and ultrasonic stirring. The GNPs embedded into the magnesium matrix led to significant enhancement in the hardness, tensile strength and ductility of the composites compared to those of unreinforced AZ91 alloy. The strength enhancement was predominantly attributed to the grain refinement by the GNP addition and dislocation generation strengthening due to the coefficient of thermal expansion mismatch between the matrix and reinforcement. The improved ductility was attributed to the refinement of β eutectics by transforming from lamellar to the divorced eutectics due to the GNP additions. In addition, the strengthening efficiency of the composite with 0.25 wt.% GNP was found to be higher than those of the composite with 0.5 wt.% GNP as the agglomeration tendency of GNPs is increased with increasing GNP content. These results were compared with those of the GNP-reinforced magnesium composites reported in the literature, indicating the potential of the process introduced in this study in terms of fabricating light and high-performance metal matrix composites.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Study on ammonia and dimethyl ether oxidation and kinetic interaction up to 100 atm

NH 3 and DME dual fuel oxidation and kinetic coupling are experimentally studied by using a supercritical pressure jet-stirred reactor (SP-JSR) at 20 and 100 atm, over a temperature range of 500–900 K, and at fuel-lean and stoichiometric conditions with NH 3 to DME molar ratios of 4 and 0.62, respectively. An HP-Mech model for high-pressure NH3/DME oxidation is developed based on our previous studies and it shows generally better performance than other models in the literature on high-pressure oxidation experiments. Due to DME’s strong low-temperature reactivity, it dramatically enhances the oxidation of NH3 at low temperature. However, the effect of NH 3 on DME oxidation varies with temperature. At low temperatures, NH 3 inhibits low-temperature reactivity by consuming OH radicals. In addition, the NH 2 and NO x formation from NH 3 further suppresses the low-temperature DME reactivity by reducing alkylperoxyl and O 2 QOOH radicals via RO 2 + NH 2 = RO + H 2 NO, RO 2 + NO = RO + NO 2 and O 2 QOOH + NO = 2CH 2 O + HO 2 + NO 2 . At intermediate temperatures, due to enhanced kinetic coupling of NH 2 /NO x /HO 2 chemistry, DME oxidation is significantly promoted. It is found that there are two major NH 2 /NO x /HO 2 coupling pathways for OH radical production brought by NH 3 : (1) NH 2 + HO 2 = H 2 NO + OH and (2) NH 2 + NO 2 = H 2 NO + NO with NO + HO 2 = OH + NO 2 . Moreover, the resulting H 2 NO will further contribute to OH production via the H 2 NO/NO x /HONO coupling pathways: H 2 NO + NO 2 = HNO + HONO, HNO + NO 2 = HONO + NO, and HONO (+M) = OH + NO (+M). These new NH 2 /NO x /HO 2 and H 2 NO/NO x /HONO pathways play a critical role in promoting DME oxidation at intermediate temperatures. Novelty and Significance Statement: Blending NH 3 with DME can significantly enhance the reactivity of NH 3 and facilitate its practical application in advanced internal combustion engines. NH 3 /DME oxidation is studied in a novel supercritical pressure jet-stirred reactor up to 100 atm, a much higher pressure than previous studies. An interesting non-monotonic effect of NH3 addition on fuel oxidation has been found. Unique kinetic couplings of NH2/HO2/NOx and H2NO/NOx/HONO brough by NH3 and DME blending are identified to play important roles in radical generation and reactivity promotion. The valuable experimental data and key kinetics revealed in the current work can tremendously improve our understanding of NH 3 /DME oxidation via NO x /RO 2 and NH 2 / H 2 NO/HO 2 /NO x kinetic couplings at low to intermediate temperatures.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2016

Microstructure evolution and mechanical properties of nano-SiCp/AZ91 composite processed by extrusion and equal channel angular pressing (ECAP)

Nano-SiCp/AZ91 magnesium matrix composite was fabricated by stir casting. The as-cast ingots were extruded at 350 °C, then processed by equal channel angular pressing (ECAP) at various temperatures (250 °C, 300 °C and 350 °C). Grains are significantly refined after the extrusion and the ECAP. A basal fibre texture was detected by neutron diffraction after the extrusion, which inclines about 45° to the extrusion direction (ED) after the ECAP. Nano-scaled SiC particles agglomerate in the as-cast composite. After the extrusion, the agglomeration tends to form continuous or discontinuous strips along the extrusion direction. By application of the ECAP, the agglomerated SiC particles are partly dispersed and the strips formed during the extrusion tend to be thinner and broken with the increasing pass number. The yield tensile strength (YTS) and the ultimate tensile strength (UTS) of the composite are dramatically increased after the extrusion. ECAP for one pass at various temperatures further increases the strength, however, the YTS decreases with the increasing ECAP temperature and the pass number. The Orowan equations predict the maximum YTS of the composite may be up to 400 MPa providing SiC particles are homogenously distributed in the matrix. - Highlights: •Nano-scaled SiC particles were successfully added into AZ91 by stirring casting. •Agglomeration of nano-particles were improved by extrusion and ECAP. •Yield strength of the composite is 328 MPa after one pass of ECAP. •Further ECAP process with optimized parameters may fully disperse nano-particles. •Yield strength is predicted to up to 400 MPa when particles are fully dispersed.

36 MATERIALS SCIENCE↗

DOE OSTI2014

Taylor-Couette flow of unmagnetized plasma

Differentially rotating flows of unmagnetized, highly conducting plasmas have been created in the Plasma Couette Experiment. Previously, hot-cathodes have been used to control plasma rotation by a stirring technique [C. Collins et al., Phys. Rev. Lett. 108, 115001 (2012)] on the outer cylindrical boundary—these plasmas were nearly rigid rotors, modified only by the presence of a neutral particle drag. Experiments have now been extended to include stirring from an inner boundary, allowing for generalized circular Couette flow and opening a path for both hydrodynamic and magnetohydrodynamic experiments, as well as fundamental studies of plasma viscosity. Plasma is confined in a cylindrical, axisymmetric, multicusp magnetic field, with T{sub e} < 10 eV, T{sub i} < 1 eV, and n{sub e}<10{sup 11} cm{sup −3}. Azimuthal flows (up to 12 km/s, M = V∕c{sub s} ∼ 0.7) are driven by edge J × B torques in helium, neon, argon, and xenon plasmas, and the experiment has already achieved Rm ∼ 65 and Pm∼0.2−12. We present measurements of a self-consistent, rotation-induced, species-dependent radial electric field, which acts together with pressure gradient to provide the centripetal acceleration for the ions. The maximum flow speeds scale with the Alfvén critical ionization velocity, which occurs in partially ionized plasma. A hydrodynamic stability analysis in the context of the experimental geometry and achievable parameters is also explored.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

DOE OSTI2019

Update on Investigations of Viability of Cold Spray and FSW as a Spent Nuclear Fuel Dry Storage Canister Mitigation Tool

The purpose of this work is to investigate the use of cold spray and friction stir welding or processing (FSW/P) for repair and mitigation of chloride-induced stress corrosion cracking (CISCC) in dry cask storage system (DCSS) canisters to ensure integrity far beyond their original license period. This report provides a viability analysis of cold spray and friction stir welding for repair and fabrication of DCSS canisters. This report presents experimental work and a research strategy to optimize and evaluate cold spray and FSW/P for CISCC resistance. The literature reports that the following three conditions must exist for CISCC to occur: tensile stress, corrosive environment, and susceptible material. These conditions must be understood and accounted for while evaluating CISCC susceptibility. Furthermore, non-obvious factors, such as surface conditions and geometric confinement, can dramatically increase the intensity of one or more of the three listed conditions for CISCC. Arc welding should be considered for either temporary or permanent repair when combined with a mitigation technology. It is known that alloys used in the existing inventory of spent nuclear fuel storage canisters become sensitized in areas around fusion welds. Technologies, such as cold spray or FSW, can mitigate the sensitization caused by fusion welds. FSW/P and cold spray, potential alternatives for fabrication and repair, are solid-phase processes. No melting occurs and the energy input can be controlled such that no harm is done to the base metal during these processes. FSW/P should be considered for use in new fabrication of canisters and repair of existing canisters. Low heat input and grain refinement result in material with improved mechanical properties and comparable generalized corrosion performance relative to base metal. FSW/P offers the potential of through-thickness CISCC resistance. Cold spray should be considered for production, mitigation, and repair of canisters. Cold spray has demonstrated the ability to deposit stainless steel, Inconel alloys, and other alloys on stainless steel 304L such that galvanic potential is matched and resistance to pitting is improved. The technical basis for cold spray mitigation and repair within the overpack using remote robotic equipment is established. A non-obvious application to the research community is the sealing of crevices. All reported instances of CISCC in the fielded nuclear applications were associated with crevice corrosion. This can be avoided by cold spraying to seal crevices. The bulk of the work planned for FY 2020 will be generating coupons for CISCC testing by collaborative projects at Pacific Northwest National Laboratory and Sandia National Laboratories. First an exploratory study will be executed that will include screening studies and process optimization. This task will identify the effect of process parameters on microstructure and CISCC resistance. Optimized parameters will be used to produce a smaller number of coupons for full testing and evaluation. Test methods for evaluating CISCC resistance must meet the following criteria: (1) normalized surface geometry and exposed process microstructure, (2) account for residual stresses, (3) be in a controlled and appropriate test environment, and (4) be numerically quantifiable and repeatable. Failure to meet these criteria could lead to results that cannot be used for comparative analysis of processes and materials.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2024

Materials Characterization, Prediction and Control Project: Summary Report on Data Analytics Framework

This report summarizes the activities performed under the data analytics Vertex in the Materials Characterization, Prediction and Control Project funded under laboratory directed research and development at Pacific Northwest National Laboratory. The data analytics Vertex developed models for associating global or local process parameters, microstructural features, and performance properties of friction-stir-processed 316L stainless steel plates. Statistical, machine learning, and deep learning models, as well as generative artificial intelligence approaches, were used to develop the associations between the process-structure-property data streams. These associations formed the basis for predicting global properties of parts manufactured under different process envelopes, providing a basis for predicting performance using data driven as well as physics-informed and physics-constrained approaches. Additionally, the associations were used to predict local process parameters and microstructural features of the product, predictive relationships that have the potential to form the basis of a control framework that could eventually modulate a friction-stir process to maintain product quality.

316L stainless steel↗

DOE OSTI2017

Giant Planets Can Act as Stabilizing Agents on Debris Disks

We have explored the evolution of a cold debris disk under the gravitational influence of dwarf-planet-sized objects (DPs), both in the presence and absence of an interior giant planet. Through detailed long-term numerical simulations, we demonstrate that when the giant planet is not present, DPs can stir the eccentricities and inclinations of disk particles, in linear proportion to the total mass of the DPs; on the other hand, when the giant planet is included in the simulations, the stirring is approximately proportional to the mass squared. This creates two regimes: below a disk mass threshold (defined by the total mass of DPs), the giant planet acts as a stabilizing agent of the orbits of cometary nuclei, diminishing the effect of the scatterers; above the threshold, the giant contributes to the dispersion of the particles.

79 ASTRONOMY AND ASTROPHYSICS↗

DOE OSTI2013

Study on the kinetics and mechanism of Am(III) with TODGA

The removal of minor actinides (mainly Am, Cm and Np) from the high-level waste would remarkably reduce the necessary storage time. Recently developed, a tridentate ligand, N,N,N',N'-tetraoctyl diglycolamide (TODGA), has been identified as one of the most powerful extractants being considered for the partitioning of trivalent actinides and lanthanides. In the present paper, the extraction kinetics behavior of Am(III) in TODGA/n-dodecane-HNO{sub 3} system has been studied, dependent on various parameters such as the stirring speed, the interfacial area, the extractant concentration in n-dodecane, the extracted ions concentration, the acidity of aqueous phase and the temperature. The results show that: the extraction process is controlled by diffusion mode under 130 rpm of stirring speed and by chemical reaction mode above 150 rpm. The extraction rate equation is given in the paper and the apparent extraction rate constant of Am(III) by TODGA/n-dodecane in 170 rpm and at 25 Celsius degrees is k=(24.2±3.4)*10{sup -3} mol{sup -2.18}*L{sup 2.18}*min{sup -1}*cm. The initial extraction rate of Am(III) by TODGA/n-dodecane at 170 r/min and 25 Celsius degrees increases with increasing temperature, and the apparent active energy is calculated to be E{sub a}=(25.94±0.98) kJ/mol.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2018

Microstructural Characterization of Al 4 C 3 in Aluminum-Graphite Composite Prepared by Electron-Beam Melting

We prepared graphite infused aluminum composites by electron-beam vacuum melting and electromagnetic stirring with 0% and 4wt% graphite addition. Bulk density of 2.69 g/cm 3 was measured for samples with 0% graphite addition (AlCv0) and 2.66 g/cm 3 for samples with 4 wt% graphite addition (AlCv4). Both are >99% of their theoretical values. X-ray diffraction indicated that AlCv0 is phase pure, while the AlCv4 sample is a composite consisting of aluminum, Al 4 C 3 , and graphite. Electron microscopy and energy dispersive X-ray spectroscopy revealed pockets of carbon rich phase of 10 to 50 μm in sizes dispersed in the Al matrix in AlCv4. Scanning transmission electron microscopy (STEM) showed that Al 4 C 3 crystallites of 1-2 μm sizes that are mostly located near the outer shell of the pockets of carbon rich phase and with undissolved graphite at the center. Thermal conductivity of 107.8 W/m·K was measured for the AlCv4 and 226.7 W/m·K for the AlCv0. Our work demonstrated the feasibility of producing pore-free high density graphite infused aluminum composite materials by electron-beam melting and electromagnetic stirring in vacuum.

36 MATERIALS SCIENCE↗

DOE OSTI2015

Grain-Size Based Additivity Models for Scaling Multi-rate Uranyl Surface Complexation in Subsurface Sediments

This study statistically analyzed a grain-size based additivity model that has been proposed to scale reaction rates and parameters from laboratory to field. The additivity model assumed that reaction properties in a sediment including surface area, reactive site concentration, reaction rate, and extent can be predicted from field-scale grain size distribution by linearly adding reaction properties for individual grain size fractions. This study focused on the statistical analysis of the additivity model with respect to reaction rate constants using multi-rate uranyl (U(VI)) surface complexation reactions in a contaminated sediment as an example. Experimental data of rate-limited U(VI) desorption in a stirred flow-cell reactor were used to estimate the statistical properties of multi-rate parameters for individual grain size fractions. The statistical properties of the rate constants for the individual grain size fractions were then used to analyze the statistical properties of the additivity model to predict rate-limited U(VI) desorption in the composite sediment, and to evaluate the relative importance of individual grain size fractions to the overall U(VI) desorption. The result indicated that the additivity model provided a good prediction of the U(VI) desorption in the composite sediment. However, the rate constants were not directly scalable using the additivity model, and U(VI) desorption in individual grain size fractions have to be simulated in order to apply the additivity model. An approximate additivity model for directly scaling rate constants was subsequently proposed and evaluated. The result found that the approximate model provided a good prediction of the experimental results within statistical uncertainty. This study also found that a gravel size fraction (2-8mm), which is often ignored in modeling U(VI) sorption and desorption, is statistically significant to the U(VI) desorption in the sediment.

Zhang, Xiaoying↗

DOE OSTI2024

A non-melting additive approach to structural repair of aluminum aircraft fastener holes

The damage to fastener holes in aerospace aluminum structures presents significant challenges for aircraft durability, and conventional bushing methods for repairing oversized holes often fall short due to the lack of metallurgical bonding and limited edge distance availability. This study investigates additive friction stir deposition, a non-melting additive process, as a viable alternative for the structural repair of aerospace fastener holes. The repair process, demonstrated on AA7050 (Al-Zn-Mg-Cu-Zr) hole structures, involves filling oversized holes with new material and machining to restore the original hole size. The repaired hole coupons are defect-free and exhibit good fatigue performance under fully reversed tension-compression loading (R = -1). At a nominal stress amplitude of 123.5 MPa, the average number of cycles to failure is 12,666 for unrepaired baseline coupons and 17,372 for effectively repaired coupons. Restoring complex geometries without compromising fatigue performance has been difficult in aerospace applications; this study marks the first demonstration of additive repair that consistently outperforms the unrepaired baseline coupons. Notably, the result is achieved through a low-energy, cost-effective solution without the need for post-repair heat treatment. Except for a few outliers, the post-repair fatigue performance generally remains inferior to that of undamaged, pristine coupons, likely due to precipitate evolution in AA7050 caused by the thermomechanical processing nature of additive friction stir deposition. This evolution weakens the repair region and the adjacent base material, leading to faster crack initiation and growth compared to the properly aged base material, AA7050-T7451.

36 MATERIALS SCIENCE↗

DOE OSTI2021

The effects of process parameters on the properties of manganese-rich carbonate precursors: A study of co-precipitation synthesis using semi-batch reactors

The synthesis of precursors for lithium- and manganese-rich xLi 2 MnO 3 ∙ (1-x)LiMO 2 (M = Ni, Mn, Co) (LMR-NMC) materials is generally carried out via co-precipitation using a continuously stirred tank reactor (CSTR) under steady-state conditions. But during the early stages of research (e.g., when screening compositional spaces of interest), using a CSTR in steady-state mode can be time consuming and wasteful. An alternative is to operate the reactor in semi-batch mode, which shortens reaction times and reduces the amount of waste. However, the effect of this mode on the product is not well documented. The present work investigates how several process variables affect the physical properties of Mn-rich NMC carbonate precursors prepared under semi-batch operation of a CSTR. The process variables examined are pH, ammonia concentration of feed solution, process temperature, stirring speed, and reaction time. Overall, the results can help guide research-scale production to support efficient development of Mn-rich carbonates for cathode oxides.

25 ENERGY STORAGE↗