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At least 1,261 records · Page 70

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NASA NTRS1997

Fiber-Optic Temperature Sensor Using a Thin-Film Fabry-Perot Interferometer

A fiber-optic temperature sensor was developed that is rugged, compact, stable, and can be inexpensively fabricated. This thin-film interferometric temperature sensor was shown to be capable of providing a +/- 2 C accuracy over the range of -55 to 275 C, throughout a 5000 hr operating life. A temperature-sensitive thin-film Fabry-Perot interferometer can be deposited directly onto the end of a multimode optical fiber. This batch-fabricatable sensor can be manufactured at a much lower cost than can a presently available sensor, which requires the mechanical attachment of a Fabry-Perot interferometer to a fiber. The principal disadvantage of the thin-film sensor is its inherent instability, due to the low processing temperatures that must be used to prevent degradation of the optical fiber's buffer coating. The design of the stable thin-film temperature sensor considered the potential sources of both short and long term drifts. The temperature- sensitive Fabry-Perot interferometer was a silicon film with a thickness of approx. 2 microns. A laser-annealing process was developed which crystallized the silicon film without damaging the optical fiber. The silicon film was encapsulated with a thin layer of Si3N4 over coated with aluminum. Crystallization of the silicon and its encapsulation with a highly stable, impermeable thin-film structure were essential steps in producing a sensor with the required long-term stability.

Beheim, Glenn↗

NASA NTRS1999

Compositions of Mars Rocks: SNC Meteorites, Differentiates, and Soils

The 13 samples from Mars identified in the terrestrial meteorite collections vary from dunite to pyroxenite to microgabbro or basalt. All of these rocks appear to have formed from primitive melts with similar major element compositional characteristics; i.e., FeO-rich and Al2O3-Poor melts relative to terrestrial basalt compositions. Although all of the SNC rocks can be derived by melting of the same Al-depleted mantle, contamination of SNC's by a Rb-enriched mantle or crustal source is required to explain the different REE characteristics of SNC rocks. Thus, there are indications of an old crustal rocktype on Mars, and this rock does not appear to have been sampled. This paper focuses primarily on the composition of the SNC basalts, however, and on the compositions of rocks which could be derived from SNC basaltic melt by magmatic processes. In particular, we consider the possible compositions which could be achieved through accumulation of early-formed crystals in the SNC primitive magma. Through a set of experiments we have determined (1) melt (magma) compositions which could be produced by melt evolution as crystals are removed from batches of this magma cooling at depth, and (2) which evolved (Si02enriched, MgO-depleted) rock compositions could be produced from the SNC magma, and how these compare with the Pathfinder andesite composition. Finally, we compare the SNC magma compositions to the Mars soil composition in order to determine whether any source other than SNC is required.

Rutherford, M. J.↗

DOE OSTI2023

Implementation of a High-Fidelity Interface Resolving Method in Nek5000

The development and utilization of computational fluid dynamics (CFD) models for large, high-temperature electric melters in the Waste Treatment and Immobilization Plant (WTP) in eastern Washington State have proven to be valuable for various purposes. These models allow for a better understanding of the physio-chemical processes occurring within the melter vessels and can contribute to improving operational efficiency, throughput, and addressing operational issues related to vitrification. The CFD models employed for these melter vessels incorporate multiphase fluid flow and heat transfer simulations in different regions, including the plenum, cold cap, and molten glass regions. As the tank waste and glass formers are introduced into the melter, a reacting batch layer known as the cold cap forms on top of the molten glass. To enhance the melt rate, forced convection bubblers located at the bottom of the melters generate convection currents that help homogenize the molten glass and provide heat to the cold cap. As the bubbles rise through the highly viscous glass, they adopt a spherical-cap shape [1]. Meanwhile, the conversion of the batch to glass generates significant amounts of gases (such as water vapor, carbon dioxide, sulfur dioxide, and NOx) due to thermal decomposition [2]. These gases become trapped between the cold cap and molten glass, forming a foam layer [3]. For modeling multiphase flow in CFD and heat transfer simulations of waste glass melters at different scales, efforts are underway to augment the capabilities of the Nek5000 [4] and NekRS [5] open-source codes [6]. Nek5000/NekRS is a scalable and efficient spectral element code that has been successfully applied to a wide range of fluid dynamics problems. By leveraging the Nek5000/NekRS software, it becomes possible to model the melter systems more affordably and with lower computational requirements compared to currently utilized commercial CFD software. The specific objectives of this ongoing effort include: 1. Implementation of a level set method in Nek5000/NekRS: The level set method is a numerical technique commonly employed in CFD simulations to track and represent the interface between different phases or materials accurately. By incorporating this method into Nek5000/NekRS, the ability to simulate multiphase flows in waste glass melters at a high level of fidelity can be achieved. 2. Demonstration of capability for air bubbling through molten glass: As part of the development process, a specific case of air bubbling through molten glass will be simulated using the augmented Nek5000/NekRS code. This demonstration aims to showcase the ability of the software to accurately capture and analyze the complex phenomena involved in the multiphase flow within waste glass melters. By achieving these objectives, the improved Nek5000/NekRS code will offer a powerful computational tool for simulating and analyzing waste glass melter systems, enabling better understanding, optimization, and troubleshooting of these vitrification processes. The ability to accurately model and simulate multiphase flows has broad relevance across many industries and scientific domains, and the improved functionality can contribute to advancements in various fields beyond waste glass melter simulations.

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DOE OSTI2023

xSDK-batched Subcontract - Ginkgo Batched Iterative Solver Development (Final Report)

Iterative solvers are fundamentally different from direct solvers in terms of execution as they generally do not execute a pre-defined sequence of operations or steps, but adapt the number of iterations to the specific problem and the preset solution quality. Generally, the adaptation of the iteration count to the problem is realized by monitoring the solver convergence and stopping the iteration process once the monitored metric, e.g., the residual norm, hits a pre-defined threshold. When addressing a set of problems with different properties, it is necessary to monitor the threshold for each problem individually and break up the SIMD execution style to avoid excess iterations for “easier” problems. Ginkgo integrates a simple but customizable stopping criterion for the residual norm and generally uses a pre-defined (relative or absolute) residual norm as the stopping criterion. In order to avoid the overhead of launching a kernel at every iteration, the iteration convergence and iteration control is part of the solver kernel. Each thread maintains its own copy of the iteration count.

97 MATHEMATICS AND COMPUTING↗

DOE OSTI2016

Defense Waste Processing Facility (DWPF) Durability-Composition Models and the Applicability of the Associated Reduction of Constraints (ROC) Criteria for High TiO 2 Containing Glasses

Radioactive high-level waste (HLW) at the Savannah River Site (SRS) has successfully been vitrified into borosilicate glass in the DWPF since 1996. Vitrification requires stringent product/process (P/P) constraints since the glass cannot be reworked once it has been poured into ten foot tall by two foot diameter canisters. A unique “feed forward” statistical process control (SPC) was developed for this control rather than relying on statistical quality control (SQC). In SPC, the feed composition to the DWPF melter is controlled prior to vitrification. In SQC, the glass product would be sampled after it is vitrified. Individual glass property-composition models form the basis for the “feed forward” SPC. The models transform constraints on the melt and glass properties into constraints on the feed composition going to the melter in order to determine, at the 95% confidence level, that the feed will be processable and that the durability of the resulting waste form will be acceptable to a geologic repository. The DWPF SPC system is known as the Product Composition Control System (PCCS). One of the process models within PCCS is known as the Thermodynamic Hydration Energy Reaction MOdel (THERMO™). The DWPF will soon be receiving increased concentrations of TiO 2 -, Na 2 O-, and Cs 2 O-enriched wastes from the Salt Waste Processing Facility (SWPF). The SWPF has been built to pretreat the high-curie fraction of the salt waste to be removed from the HLW tanks in the F- and H-Area Tank Farms at the SRS. In order to validate the existing TiO 2 term in THERMO™ beyond 2.0 wt% in the DWPF, new durability data were developed over the target range of 2.00 to 6.00 wt% TiO 2 and evaluated against the 1995 durability model. The durability was measured by the 7-day Product Consistency Test. This study documents the adequacy of the existing THERMO™ terms. It is recommended that the modified THERMO™ durability models and the modified property acceptable region limits for the durability constraints be incorporated in the next revision of the technical bases for PCCS and then implemented into PCCS. It is also recommended that an reduction of constraints of 4 wt% Al 2 O 3 be implemented with no restrictions on the amount of alkali in the glass for TiO 2 values ≥2 wt%. The ultimate limit on the amount of TiO 2 that can be accommodated from SWPF will be determined by the three PCCS models, the waste composition of a given sludge batch, the waste loading of the sludge batch, and the frit used for vitrification.

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DOE OSTI2019

Implementation of Ion Exchange Processes on Industrial Waste Streams for CO 2 Mineralization

Economic development and population growth will lead to an increase in global energy consumption. Large coal-fired power plants (>500 MW) account for almost half of the total CO 2 emissions from fossil fuel combustion, and nearly 26% of the global fossil fuel and industry CO 2 emissions. Long-term management of the more than 36 Gt of CO 2 that is emitted globally per year is urgently needed. CO 2 mineralization is an attractive method of sequestering CO 2 because it captures CO 2 as an insoluble carbonate mineral, mimicking the natural process of rock weathering. Here, we present a pathway for accelerated CO 2 mineralization enabled by divalent cations sourced from liquid streams. In this work, we investigate a mineralization route that converts flue gas CO 2 to precipitated calcium carbonate (PCC) using waste aqueous streams as the calcium source. The proposed mineralization route integrates CO 2 utilization and waste liquid management at coal power plants. Maintaining alkalinity during carbonation is the primary challenge in this process. Instead of relying on the consumption of costly and unsustainable sources of alkalinity (e.g., sodium hydroxide), we used regenerable solids to increase the pH of water by ion exchange. The increase in alkalinity creates a more thermodynamically favorable environment for calcite precipitation. The capacities for ion exchange of various commercially available zeolites and ion exchange resins in CO 2 -saturated water were studied through batch equilibrium and column ion-exchange experiments. During ion exchange, H + in the water exchanges with Na + , Ca 2+ or K + in the zeolite or resin. Batch equilibrium isotherms for H + –Na + exchange were collected by first adding varying amounts of the ion exchange solid (0 – 1.0 kg per kg of water) to CO 2 -saturated water (pCO 2 = 1 atm, pH 4) to determine the maximum H + –Na + exchange achievable. Ion-exchange column studies were performed to determine breakthrough capacity of the system. In both systems, an increase in pH coupled with an increase in Na concentration was observed, demonstrating the feasibility of forward ion exchange. Zeolitic materials increased the alkalinity of the solution from pH 4 to around 10, whereas ion exchange resins containing weakly acidic functional groups (e.g., carboxylic acid) exhibited higher affinity for H + , increasing pH to 11.3 and surpassing the pH shift induced by the zeolitic materials. The extent of calcite precipitation was evaluated by mixing the alkaline CO 3 2- -rich water obtained after passing through the ion-exchange column and a CaCl 2 solution. Calcite yields are as expected from chemical thermodynamics. Calcium carbonate yields found experimentally were about 26 and 8 mmol per kg water for the weakly acidic ion exchange resin and zeolitic materials, respectively. The results from these studies indicate that ion exchange processes can be used as an alternative to the addition of stoichiometric inorganic bases (e.g., sodium hydroxide) to induce alkalinity for the consequent precipitation of CaCO 3 . Instead, weakly acidic ion exchange resins commonly used for water hardness removal were alternatively used to induce pH swings in the aqueous solutions. The high calcium carbonate yields obtained for the materials examined demonstrate the potential application of this process. In addition, the successful operation of the calcium carbonate production process at standard temperature and pressure conditions support its potential for industrial implementation.

Simonetti, Dante↗

DOE OSTI2015

Biotransformation of furanic and phenolic compounds with hydrogen gas production in a microbial electrolysis cell

In this study, furanic and phenolic compounds are problematic byproducts resulting from the decomposition of lignocellulosic biomass during biofuel production. This study assessed the capacity of a microbial electrolysis cell (MEC) to produce hydrogen gas (H 2 ) using a mixture of two furanic (furfural, FF; 5-hydroxymethyl furfural, HMF) and three phenolic (syringic acid, SA; vanillic acid, VA; and 4-hydroxybenzoic acid, HBA) compounds as the sole carbon and energy source in the bioanode. The rate and extent of biotransformation of the five compounds, efficiency of H 2 production, as well as the anode microbial community structure were investigated. The five compounds were completely transformed within 7-day batch runs and their biotransformation rate increased with increasing initial concentration. At an initial concentration of 1,200 mg/L (8.7 mM) of the mixture of the five compounds, their biotransformation rate ranged from 0.85 to 2.34 mM/d. The anode coulombic efficiency was 44-69%, which is comparable to wastewater-fed MECs. The H 2 yield varied from 0.26 to 0.42 g H 2 -COD/g COD removed in the anode, and the bioanode volume-normalized H 2 production rate was 0.07-0.1 L/L-d. The major identified fermentation products that did not transform further were catechol and phenol. Acetate was the direct substrate for exoelectrogenesis. Current and H 2 production were inhibited at an initial substrate concentration of 1,200 mg/L, resulting in acetate accumulation at a much higher level than that measured in other batch runs conducted with a lower initial concentration of the five compounds. The anode microbial community consisted of exoelectrogens, putative degraders of the five compounds, and syntrophic partners of exoelectrogens. The H 2 production route demonstrated in this study has proven to be an alternative to the currently used process of reforming natural gas to supply H 2 needed to upgrade bio-oils to stable hydrocarbon fuels.

08 HYDROGEN↗

DOE OSTI2025

Round Robin Measurements of Molten Salt Properties for LiF-NaF-KF (FLiNaK) and NaCl-KCl Mixtures

The development, operation, and regulation of nuclear reactors that utilize molten salts as fuel or as heat transfer media require knowledge of the thermal properties of the salt systems and quantification of the corresponding uncertainties. Knowledge of molten salt properties is also necessary for applications in material synthesis, processing, separations, solar thermal power generation, and energy storage. A round robin was conducted with national laboratory and university participants from twenty-one laboratories in five countries to compare property measurements, to better understand uncertainties, and to identify possible best practices. Two salt mixtures, each from a common batch, were distributed to participants for evaluation: equimolar NaCl-KCl and 45.0LiF-13.7NaF-41.3KF mol % (FLiNaK). Measurements were performed to determine the major constituent composition, oxygen content, density, thermal expansivity, melting point, and thermal conductivity. Error analysis was performed on each measurement for uncertainty quantification for each type of property that was explored. Finally, the resulting discussion of the methodologies used in this work is meant to lay the groundwork for the development of standard methods and reference materials for future high-temperature property measurements on halide melts.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2023

Tolerance of engineered Rhodosporidium toruloides to sorghum hydrolysates during batch and fed-batch lipid production

Abstract Background Oleaginous yeasts are a promising candidate for the sustainable conversion of lignocellulosic feedstocks into fuels and chemicals, but their growth on these substrates can be inhibited as a result of upstream pretreatment and enzymatic hydrolysis conditions. Previous studies indicate a high citrate buffer concentration during hydrolysis inhibits downstream cell growth and ethanol fermentation in Saccharomyces cerevisiae . In this study, an engineered Rhodosporidium toruloides strain with enhanced lipid accumulation was grown on sorghum hydrolysate with high and low citrate buffer concentrations. Results Both hydrolysis conditions resulted in similar sugar recovery rates and concentrations. No significant differences in cell growth, sugar utilization rates, or lipid production rates were observed between the two citrate buffer conditions during batch fermentation of R. toruloides . Under fed-batch growth on low-citrate hydrolysate a lipid titer of 16.7 g/L was obtained. Conclusions Citrate buffer was not found to inhibit growth or lipid production in this engineered R. toruloides strain, nor did reducing the citrate buffer concentration negatively affect sugar yields in the hydrolysate. As this process is scaled-up, $131 per ton of hydrothermally pretreated biomass can be saved by use of the lower citrate buffer concentration during enzymatic hydrolysis. Graphical Abstract

09 BIOMASS FUELS↗

DOE OSTI2019

Report on Assessment of Advanced Reactor Fuel Performance

Three activities have been performed in FY 2019 to support the Advanced Fuel Cycle Campaign, which include assessment of annular fuel performance in an ultra-high burnup sodium-cooled reactor (SFR), modeling of annular fuel behavior during a transient scenario, and feasibility of a sustainable closed fuel cycle utilizing melt-refining process. Annular fuel performance parameters, including temperature profile, swelling strain, and cumulative damage fraction (CDF), in a 3000 MWt Sustainable Sodium-cooled Fast Reactor (SSFR) were assessed using the BISON fuel performance code. The SSFR is once-through ultra-long-life core based on a 34-batch fuel management scheme with 1.5-year cycle length. The fuel residence time in the SSFR is 51 years and the average discharged burnup is about 30%. Annular fuel has potential to irradiate for ultra-high burnup without major fuel-cladding mechanical interaction. This feature is achieved by using a low smeared density (~55%). In the SSFR design, however, 75% smeared density and a thick fuel pin were preferred to maintain criticality for 51 years. Due to the high smeared density and thick fuel pin configuration, the annular fuel was predicted to suffer premature cladding failure before reaching the discharge burnup of the SSFR. The current fuel creep model predicts a prominent creep strain due to gravity over the half-century irradiation, which may significantly affect the evolution of CDF. Thus, in order to use the annular fuel in an ultra-high burnup core such as the SSFR, a low smeared density and thin annular fuel is strongly recommended.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2026

Evaluation of Pu Solubility in Glass for Sludge Batch 11

Stainless-steel clad Pu from Japan’s Fast Critical Assembly (FCA) reactor is currently being dispositioned at the Savannah River Site. The electrolytic dissolver, operated by Savannah River Nuclear Solutions in H-Canyon, is being utilized to dissolve the material. The resulting solutions are transferred to the Concentration, Storage, and Transfer Facilities, operated by Savannah River Mission Completion (SRMC), for subsequent vitrification at the Defense Waste Processing Facility (DWPF). In support of the FCA mission startup, a preliminary evaluation was conducted by the Savannah River National Laboratory to assess the impact of the FCA discards on the liquid waste system.

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NASA NTRS1976

A simulation of water pollution model parameter estimation

A parameter estimation procedure for a water pollution transport model is elaborated. A two-dimensional instantaneous-release shear-diffusion model serves as representative of a simple transport process. Pollution concentration levels are arrived at via modeling of a remote-sensing system. The remote-sensed data are simulated by adding Gaussian noise to the concentration level values generated via the transport model. Model parameters are estimated from the simulated data using a least-squares batch processor. Resolution, sensor array size, and number and location of sensor readings can be found from the accuracies of the parameter estimates.

Kibler, J. F.↗

NASA NTRS1978

MBASIC batch processor architectural overview

The MBASIC (TM) batch processor, a language translator designed to operate in the MBASIC (TM) environment is described. Features include: (1) a CONVERT TO BATCH command, usable from the ready mode; and (2) translation of the users program in stages through several levels of intermediate language and optimization. The processor is to be designed and implemented in both machine-independent and machine-dependent sections. The architecture is planned so that optimization processes are transparent to the rest of the system and need not be included in the first design implementation cycle.

Reynolds, S. M.↗

NASA NTRS2006

Single-Wall Carbon Nanotube Anodes for Lithium Cells

In recent experiments, highly purified batches of single-wall carbon nanotubes (SWCNTs) have shown promise as superior alternatives to the graphitic carbon-black anode materials heretofore used in rechargeable thin-film lithium power cells. The basic idea underlying the experiments is that relative to a given mass of graphitic carbon-black anode material, an equal mass of SWCNTs can be expected to have greater lithium-storage and charge/discharge capacities. The reason for this expectation is that whereas the microstructure and nanostructure of a graphitic carbon black is such as to make most of the interior of the material inaccessible for intercalation of lithium, a batch of SWCNTs can be made to have a much more open microstructure and nanostructure, such that most of the interior of the material is accessible for intercalation of lithium. Moreover, the greater accessibility of SWCNT structures can be expected to translate to greater mobilities for ion-exchange processes and, hence, an ability to sustain greater charge and discharge current densities.

Hepp, Aloysius F.↗

DOE OSTI2017

Mild oxidation of methane to methanol or acetic acid on supported isolated rhodium catalysts

An efficient and direct method of catalytic conversion of methane to liquid methanol and other oxygenates would be of considerable practical value. However, it remains an unsolved problem in catalysis, as typically it involves expensive or corrosive oxidants or reaction media(5-8) that are not amenable to commercialization. Although methane can be directly converted to methanol using molecular oxygen under mild conditions in the gas phase, the process is either stoichiometric (and therefore requires a water extraction step) or is too slow and low-yielding to be practical. Methane could, in principle, also be transformed through direct oxidative carbonylation to acetic acid, which is commercially obtained through methane steam reforming, methanol synthesis, and subsequent methanol carbonylation on homogeneous catalysts. However, an effective catalyst for the direct carbonylation of methane to acetic acid, which might enable the economical small-scale utilization of natural gas that is currently flared or stranded, has not yet been reported. Here we show that mononuclear rhodium species, anchored on a zeolite or titanium dioxide support suspended in aqueous solution, catalyse the direct conversion of methane to methanol and acetic acid, using oxygen and carbon monoxide under mild conditions. Here, we find that the two products form through independent pathways, which allows us to tune the conversion: three-hour-long batch-reactor tests conducted at 150 degrees Celsius, using either the zeolitesupported or the titanium-dioxide-supported catalyst, yield around 22,000 micromoles of acetic acid per gram of catalyst, or around 230 micromoles of methanol per gram of catalyst, respectively, with selectivities of 60-100 per cent. Finally, we anticipate that these unusually high activities, despite still being too low for commercial application, may guide the development of optimized catalysts and practical processes for the direct conversion of methane to methanol, acetic acid and other useful chemicals.

09 BIOMASS FUELS↗

DOE OSTI2023

Data-driven acoustic measurement of moisture content in flowing biomass

Measuring the moisture content in flowing biomass is critical to processes such as liquid biofuel conversion, such as biogasoline, biodiesel, bio jet kerosene, etc. However, biomass tends to flow in aggregates, which results in significant inhomogeneities in the amount of biomass flowing in front of a sensor at a given time, and there can be significant overlap in the material properties of dry vs wet biomass, leading to poor signal-to-noise ratio. We present a technique for identifying biomass moisture content using a series of acoustic pitch-catch measurements to quantify the sound speed and acoustic amplitude through the biomass, in conjunction with classical machine learning techniques, including Naive Bayes, Random Forest, and K-Nearest Neighbors classification. We amplify the differences between the acoustic measurements in different moisture levels by collecting a series of pulse-echo measurements, which we sort in order of ascending sound speed. We test the accuracy of the technique on experimentally-prepared batches of corn stover biomass with specified moisture levels and measure the average error in the estimated moisture level as a function of the number of pitch-catch measurements used. We observe average estimation errors as low as 6.7% by increasing the number of measurements and optimizing the hyperparameters. This work presents a novel method determining moisture content in flowing biomass with inhomogeneous flow. Additionally, this technique has application in optimizing biomass conversion processes, as well as other fields including, paper production, natural fiber processing, and mineral extraction.

09 BIOMASS FUELS↗

DOE OSTI2018

Production of monodisperse cerium oxide microspheres with diameters near 100 µm by internal-gelation sol–gel methods

Cerium dioxide microspheres with uniform diameters between 65 – 211 µm were fabricated using internal gelation sol-gel methods. Although uniform microspheres are produced for nuclear fuel applications with diameters above 300 µm, sol-gel microspheres with diameters of 50 - 200 µm have historically been made by emulsion techniques and had poor size uniformity [1, 2]. An internal gelation, sol-gel apparatus was designed and constructed to accommodate the production of small, uniform microspheres whereby cerium-containing solutions were dispersed into flowing silicone oil and heated in a gelation column to initiate solidification [3, 4]. Problems with premature feed gelation and microsphere coalescence were overcome by equipment modifications unique among known internal gelation setups. Microspheres were fabricated and sized in batches as a function of dispersing needle diameter and silicone oil flow rate in the two-fluid nozzle in order to determine the range of sizes possible and corresponding degree of monodispersity. Initial experiments with poor size uniformity were linked to microsphere coalescence in the gelation column prior to solidification as well as excessive flow rates for the cerium feed solution. Average diameter standard deviations as low as 2.23% were observed after optimization of flow rates and minimization of coalescence reactions.

cerium oxide↗

DOE OSTI2017

Investigation of zinc recovery by hydrogen reduction assisted pyrolysis of alkaline and zinc-carbon battery waste

Highlights: • Recycling of alkaline and zinc-carbon battery waste by pyrolysis. • Thermodynamic investigation for hydrogen reduction of alkaline battery waste. • Recovery of Zn as submicron particle from alkaline battery waste. • Production of manganese oxide particles from alkaline battery waste. • Controlling oxidation state of manganese oxide product in the process. - Abstract: Zinc (Zn) recovery from alkaline and zinc-carbon (Zn-C) battery waste were studied by a laboratory scale pyrolysis process at a reaction temperature of 950 °C for 15–60 min residence time using 5%H{sub 2(g)}-N{sub 2(g)} mixture at 1.0 L/min gas flow rate. The effect of different cooling rates on the properties of pyrolysis residue, manganese oxide particles, were also investigated. Morphological and structural characterization of the produced Zn particles were performed. The battery black mass was characterized with respect to the properties and chemical composition of the waste battery particles. The thermodynamics of the pyrolysis process was studied using the HSC Chemistry 5.11 software. A hydrogen reduction reaction of the battery black mass (washed with Milli-Q water) takes place at the chosen temperature and makes it possible to produce fine Zn particles by rapid condensation following the evaporation of Zn from the pyrolysis batch. The amount of Zn that can be separated from the black mass increases by extending the residence time. Recovery of 99.8% of the Zn was achieved at 950 °C for 60 min residence time using 1.0 L/min gas flow rate. The pyrolysis residue contains MnO and Mn{sub 2}O{sub 3} compounds, and the oxidation state of manganese can be controlled by cooling rate and atmosphere. The Zn particles exhibit spherical and hexagonal particle morphology with a particle size varying between 200 nm and 3 µm. However the particles were formed by aggregation of nanoparticles which are primarily nucleated from the gas phase.

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