Ultra-Fast Calcination of Lithium Ion Battery Cathode Materials
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25 ENERGY STORAGE↗
SEARCH · Engineering Papers
Results for “calcination”
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CONCENTRATED SOLAR POWER COUPLED WITH WASTE HEAT RECOVERY SYSTEM FOR INNOVATIVE CLINKER CALCINATION PROCESS
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Alvarez, Francisco↗
Synthesis of murdochite-type Ni{sub 6}MnO{sub 8} with variable specific surface areas and the application in methane oxidation
To synthesize a murdochite-type Ni{sub 6}MnO{sub 8} with variable specific surface areas, an oxalate precursor was calcined at 350–500 °C in flowing argon, and the calcined sample was heated to 600 °C in air. The lattice constant of the Ni{sub 6}MnO{sub 8} did not depend on the calcination temperature of the precursor, while the specific surface area decreased from 8.4 m{sup 2}/g to 2.6 m{sup 2}/g when increasing the calcination temperature of the precursor. The methane (CH{sub 4}) oxidation data indicated that the temperature corresponding to the 50% conversion (T{sub 50%}) of Ni{sub 6}MnO{sub 8} calcined at 350 °C or 400 °C was lower than that of all other Ni{sub 6}MnO{sub 8} specimens. However, the intrinsic conversion of Ni{sub 6}MnO{sub 8} calcined at 350 °C, which is defined as conversion per specific surface area, was half of that of all other Ni{sub 6}MnO{sub 8} specimens. The degree of crystallinity and catalytic performance of the Ni{sub 6}MnO{sub 8} calcined at 400 °C were high. - Graphical abstract: The conversion of CH{sub 4} into CO{sub 2} and H{sub 2}O on Ni{sub 6}MnO{sub 8}, which was heated at 600 °C in air after the calcination of the precursor at 350 °C, 400 °C, 450 °C, or 500 °C in flowing argon, was measured. Since the specific surface area was strongly affected by the calcination temperature of the precursor, intrinsic conversion (IC) was defined as conversion per the specific surface area. For comparison, the IC value on Ni{sub 6}MnO{sub 8} synthesized by the direct calcination of the precursor at 600 °C in air is plotted. - Highlights: • The oxalate precursor was calcined at 350–500 °C in flowing argon. • Murdochite-type Ni{sub 6}MnO{sub 8} was obtained by heating the calcined sample in air. • The specific surface area of Ni{sub 6}MnO{sub 8} varied with the calcination temperature. • The degree of crystallinity and catalysis of Ni{sub 6}MnO{sub 8} calcined at 400 °C were high.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Remote Robotic Equipment for Retrieval of High Level Waste to Support Environmental Closure - 18162
The Idaho Cleanup Project contractor, Fluor Idaho, LLC, is responsible for managing HLW calcine stored in the Calcined Solids Storage Facility at the Idaho Nuclear Technology and Engineering Center. The Idaho Nuclear Technology and Engineering Center is a DOE managed facility located at the INL Site in the remote portions of southeast Idaho. In 2016, DOE directed Fluor Idaho to develop and test a full-scale retrieval system to demonstrate the ability to safely retrieve HLW calcine from the Calcined Solids Storage Facility for future retrieval and processing. Removing HLW calcine from the State of Idaho is required by the 1995 Settlement Agreement, which mandates that DOE have HLW calcine ready to be moved out of Idaho by December 2035. Fluor Idaho is currently testing retrieval and transfer concepts to ensure that the Calcined Solids Storage Facility is placed in a final configuration that is protective of human health and the environment after HLW calcine has been removed to the maximum extent practical. This paper describes the full-scale prototype that will be used to prove retrieval and transfer system design capabilities, verify operating parameters, and establish a basis for calcine retrieval efficacy. Additionally, it describes the retrieval (bulk and residual) and visual monitoring systems that were designed and tested in 2017 and will continue to be tested with the full-scale prototype. Testing (i.e., full-scale mockup, bulk retrieval, residual clean-out, and visualization monitoring) performed by Fluor Idaho will demonstrate the maximum extent practical of HLW calcine removal that is achievable. This is critical to (1) establish criteria for ending calcine removal activities, (2) evaluate cost and benefits associated with performing additional removal, and (3) ensure clean up and closure standards under applicable requirements (e.g., statutes, orders, and agreements) are met. (authors)
12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
Waste Treatment of Acidic Solutions from the Dissolution of Irradiated LEU Targets for 99-Mo Production
One of the missions of the Reduced Enrichment for Research and Test Reactors (RERTR) program (and now the National Nuclear Security Administrations Material Management and Minimization program) is to facilitate the use of low enriched uranium (LEU) targets for 99 Mo production. The conversion from highly enriched uranium (HEU) to LEU targets will require five to six times more uranium to produce an equivalent amount of 99 Mo. The work discussed here addresses the technical challenges encountered in the treatment of uranyl nitrate hexahydrate (UNH)/nitric acid solutions remaining after the dissolution of LEU targets. Specifically, the focus of this work is the calcination of the uranium waste from 99 Mo production using LEU foil targets and the Modified Cintichem Process. Work with our calciner system showed that high furnace temperature, a large vent tube, and a mechanical shield are beneficial for calciner operation. One- and two-step direct calcination processes were evaluated. The high-temperature one-step process led to contamination of the calciner system. The two-step direct calcination process operated stably and resulted in a relatively large amount of material in the calciner cup. Chemically assisted calcination using peroxide was rejected for further work due to the difficulty in handling the products. Chemically assisted calcination using formic acid was rejected due to unstable operation. Chemically assisted calcination using oxalic acid was recommended, although a better understanding of its chemistry is needed. Overall, this work showed that the two-step direct calcination and the in-cup oxalic acid processes are the best approaches for the treatment of the UNH/nitric acid waste solutions remaining from dissolution of LEU targets for 99 Mo production.
12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
Robotic Solutions for Remote Access and Retrieval of High-Level Radioactive Waste - 19544
This paper describes the ongoing development of robotic solutions for accessing and retrieving high-level radioactive waste from underground storage bins as part of the Calcine Retrieval Project at the INL Site. The waste is in the form of a solid powder, referred to as calcine, stored in a set of stainless steel bins within an underground concrete vault. Due to the radiation field produced by the calcine, all operations must be performed remotely. The Calcine Retrieval Project is currently carrying out proof-of-concept testing of methods for the various stages of calcine retrieval. The bins were designed with no means for access, so retrieval operations will require welding access riser pipes to the bins, followed by cutting through the bin walls from within the risers. These tasks are complicated by the fact that four of the risers must be placed off center on a domed surface, resulting in a weld joint that is curved and tilted relative to the riser axis. The Access Riser Connection robot is being developed to perform these operations using interchangeable welding and plasma cutting attachments. The majority of the calcine will be removed using a vacuum system and pneumatically transferred to storage. This system is not described in this paper. However, the bins contain several internal features that are expected to retain calcine, most notably circumferential stiffening rings on the walls and radial ribs on the floors. One of the solutions being developed for the task of retrieving this residual calcine is a vacuum crawler, a wheeled robot using vacuum to adhere to the interior walls of the bins. The vacuum crawler would use a separate vacuum system to remove residual calcine or would use compressed air to move calcine to a location from which it can be retrieved more easily. While comparable welding and wall-climbing robots have been developed before, this particular application has several constraints that are not satisfied by existing systems. For this reason, both the access riser welder and the vacuum crawler, although still under development, may be of interest to other projects faced with similar constraints. (author)
12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
Synthesis of cuboid-type tungsten trioxide photocatalysts for oxygen evolution from water in the presence of silver(I) sulfate under visible light irradiation
Highlights: • Visible-light photocatalytic cuboid-type tungsten trioxide (C-WO{sub 3}) particles were prepared by calcination at various temperatures between 200 and 500 °C. • Photocatalysis of the prepared C-WO{sub 3} samples was investigated for oxygen evolution from water in the presence of sacrificial silver(I) sulfate. • The photocatalytic activity differed among the samples and the sample calcined at 400 °C showed the top activity. • The main factor influencing the photocatalytic activity of the C-WO{sub 3} was determined. - Abstract: We synthesized various cuboid-type tungsten trioxide (WO{sub 3}) particles using a hydrothermal method followed by calcination at various temperatures between 200 and 500 °C. Visible-light photocatalysis of these particles was investigated for oxygen (O{sub 2}) evolution from water in the presence of sacrificial silver(I) sulfate. The calculated crystallite diameters increased with increasing calcination temperature, suggesting that the level of crystallinity increased with calcination temperature. The average specific surface area of the particles was almost the same for all calcination temperatures in the range 200–400 °C, but was decreased at 500 °C. The photocatalytic reaction rate of O{sub 2} formation increased with increasing calcination temperature up to 400 °C, and then decreased as calcination temperature was further increased to 500 °C. We therefore concluded that the rate increased with calcination temperature up to 400 °C due to the increasing crystallinity, but then decreased due to the decreased specific surface area.
75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
Analysis of textural properties of CaO-based CO 2 sorbents by ex-situ USAXS
Here in this work, the micro-textural properties of CaO-based CO 2 sorbents prepared in a thermo-gravimetric reactor were investigated by ex situ synchrotron-based Small Angle X-ray Scattering (SAXS), Ultra Small Angle X-ray Scattering (USAXS) and Wide Angle X-ray Scattering (WAXS). Six sorbent samples were produced by calcination in vacuum at different temperatures and durations of the heating step; additionally, four partially carbonated samples were produced, after calcination in vacuum, at different CaO conversions. The scattering intensity profiles were analyzed by means of the Unified Fit model. Bimodal pore size distributions (micro-pores and meso-pores) were identified and the micro-textural properties (porosity, specific surface and pore radius of gyration) of each of the two pore populations were quantified both for the calcined and for the carbonated samples. The micro-textural properties of a few calcined samples were compared with N 2 -adsorption measurements. For each pore population, the trends of porosity, specific surface and pore radius of gyration, in addition to the pore number density and sphericity factor, were obtained versus time during the calcination and versus the CaO conversion during the carbonation. The relevance of micro-pores with respect to macro-pores was assessed both as far as the porosity impact on the CO 2 capture capacity and as far as the specific surface impact on the carbonation kinetics. For the calcined samples, the micro-textural properties of a partially calcined sample were compared with those of the completely calcined samples, and pore correlation distances were determined. Finally, for the carbonated samples, the specific surface per unit of particle volume results linearly dependent on the CaO conversion and, if expressed per unit of mass of unreacted CaO, does not change significantly for most of the CaO carbonation.
36 MATERIALS SCIENCE↗
Electrochemical and Magnetic Properties of Electrospun SrTi{sub 1−x}Fe{sub x}O{sub 3} (x = 0, 0.05 and 0.10) Nanofibers for Anodes of Li-Ion Batteries
SrTi{sub 1−x}Fe{sub x}O{sub 3} (x = 0, 0.05 and 0.1) nanofibers (NFs) were fabricated by electrospinning technique. As prepared products were calcined at 800 {sup ∘} C in argon atmosphere for 3 h to obtain a perovskite phase. The crystal structure and morphology of samples were investigated using X-ray diffraction (XRD), transmission electron microscopy (TEM) and scanning electron microscopy (SEM). Electrochemical and magnetic properties of calcined NFs were studied using a potentiostat/galvanostat electrochemical cell system and vibrating sample magnetometer (VSM), respectively. XRD results showed the cubic perovskite structure of calcined samples with the diameter estimated by TEM in the range of 137.4–141.3 nm SEM micrographs revealed the linkage of crystalline grains in NFs of porous and rough surfaces. Electrochemical properties performed on coin-cell-type Li-ion batteries (LIBs) with calcined SrTi{sub 1−x}Fe{sub x}O{sub 3} (x = 0.05 and 0.10) NF-based anodes showed a significant increase of the specific capacity from 305 to 431 mAh/g for the first cycle with the reversible values of 100 and 130 mAh/g, respectively. VSM measurements at room temperature (RT) indicated that calcined SrTiO{sub 3} NFs exhibited paramagnetic (PM) behavior, while calcined SrTi{sub 1−x}Fe{sub x}O{sub 3} NFs displayed ferromagnetic (FM) behavior at RT with the increase of unsaturated magnetization at 10 kOe from 0.46 to 0.82 emu/g for samples with x = 0.05 and 0.10, respectively. The observed FM behavior in calcined SrTi{sub 1−x}Fe{sub x}O{sub 3} (x = 0.05 and 0.1) NFs was suggested to originate from the face center exchange (FCE) mechanism owing to Fe{sup 3+} –Vo–Fe{sup 3+} couplings.
75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
Room Temperature Adsorptive Removal of Thiophene over Zinc Oxide-Based Adsorbents
This study investigated the room temperature adsorptive removal of thiophene over zinc oxide adsorbents in the presence of hydrogen. The bulk zinc oxide was prepared by precipitation method and calcined at different temperatures in the range of 300-550 °C. Supported zinc oxide was prepared by co-precipitation of 30 wt.% ZnO with alumina and calcined at 550 °C. Properties of the adsorbents were determined by various characterization techniques such as surface area and pore volume analysis, XRD, FESEM, EDX and TPR. The desulfurization process was carried out in a down-flow packed bed reactor at room temperature (30 °C). The BET surface area of bulk zinc oxide adsorbents decreased with the increase in calcination temperature from 300 to 550 °C. The surface area of bulk zinc oxide adsorbents was 30.5 and 14.6 m{sup 2}/g when calcined at 300 and 550 °C, respectively. The surface are of supported zinc oxide adsorbents was 177 m{sup 2}/g. The highest average pore size was obtained for bulk ZnO calcined at 550 °C (45 nm) compared to that calcined at 300 °C (42 nm) and supported ZnO (27 nm). The XRD peaks corresponded to the hexagonal structure of zinc oxide. The removal of thiophene was most significant for bulk ZnO calcined at 550 °C. The higher removal efficiency for this adsorbent in spite of lower surface area may be attributed to its higher percentage of larger pores and higher average pore size.
36 MATERIALS SCIENCE↗
Investigation of the thermal decomposition of Pu(IV) oxalate: a transmission electron microscopy study
The degradation of the internal structure of plutonium (IV) oxalate during calcination was investigated with Transmission Electron Microscopy (TEM), electron diffraction, Electron Energy-Loss Spectroscopy (EELS), and 4D Scanning TEM (STEM). TEM lift-outs were prepared from samples that had been calcined at 300°C, 450°C, 650°C and 950°C. The resulting phase at all calcination temperatures was identified as PuO 2 with electron diffraction. The grain size range was obtained with high-resolution TEM. In addition, 4D STEM images were analyzed to provide grain size distributions. In the 300°C calcined sample, the grains were <10 nm in diameter, at 650°C, the grains ranged from 10 to 20 nm, and by 950°C, the grains were 95–175 nm across. Using the Kolmogorov-Smirnov (K-S) two sample test, it was shown that morphological measurements obtained from 4D-STEM provided statistically significant distributions to distinguish samples at the different calcination conditions. Using STEM-EELS, carbon was shown to be present in the low temperature calcined samples associated with oxalate but had formed carbon (possibly graphite) deposits in the 950°C calcined sample. This work highlights the new methods of STEM-EELS and 4D-STEM for studying the internal structure of special nuclear materials (SNM).
11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
Thermal Desulfurization of Petroleum Coke for Anode Use
Thermal desulfurization (TDS) of petroleum coke during calcination is a well-known phenomenon which results in an increase in porosity and decrease in bulk density. Rain Carbon presented a paper recently which explored the potential of using a shaft calciner to TDS coke instead of a rotary kiln calciner. There are some significant benefits in using a shaft calciner due to the slower heat-up rate but the coke structure is still irreversibly changed when sulphur (S) is driven from the coke. This paper presents a review of the differences in TDS at different heating rates and includes high resolution scanning electron microscopy and helium ion microscopy images. The potential for TDS petroleum coke to allow a wider range of GPC raw materials to be used for anode production is discussed. At least one coke calcining company in China has attempted aggressive TDS on a production scale. High S cokes are readily available and cheaper than low S cokes and removing SO2 during calcination is more efficient than removing SO2 from potroom flue-gas streams to meet emission limits. There are significant practical limits to the level of TDS that can be tolerated however, both from a calciner’s perspective and for anode quality/performance reasons.
Edwards, Les↗
Preparation of LaB{sub 3}O{sub 6}:Eu{sup 3+} phosphors by a facile precursor method and their luminescent properties
Graphical abstract: LaB{sub 3}O{sub 6}:Eu{sup 3+} phosphor was obtained by calcining the precursor which was synthesized by boric acid melting method. It (a) exhibits much stronger PL intensity than that (b) prepared by conventional solid state reaction method. - Highlights: • A calcining precursor method was used for preparation of LaB{sub 3}O{sub 6}:Eu{sup 3+} phosphor. • Precursor was prepared by boric acid melting method. • The luminescence intensity of LaB{sub 3}O{sub 6}:Eu{sup 3+} was enhanced by the present method. - Abstract: The LaB{sub 3}O{sub 6}:Eu{sup 3+} phosphors were prepared by calcining the precursors which were synthesized by boric acid melting method using rare earth oxide and boric acid as raw materials, and they were characterized by EDS, XRD, IR, SEM and PL. The influences of reaction temperature for the preparation of precursor and subsequent calcination temperature and time of precursor on the luminescence properties of LaB{sub 3}O{sub 6}:Eu{sup 3+} phosphor were investigated. The results showed that the LaB{sub 3}O{sub 6}:Eu{sup 3+} phosphors with maximum luminescent intensity were obtained by calcining precursor at 1000 °C for 6 h, in which the precursor was prepared at 200 °C for 72 h. Compared with the conventional high temperature solid-state reaction method, the pure LaB{sub 3}O{sub 6}:Eu{sup 3+} phosphor can be obtained at relatively lower calcination temperature by the precursor method and exhibits much stronger emission intensity.
36 MATERIALS SCIENCE↗
Characterization of LaRhO3 perovskites for dry (CO2) reforming of methane (DRM)
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dry reforming of methane↗
Thermal Decomposition of Bulk K-CoMoSx Mixed Alcohol Catalyst Precursors and Effects on Catalyst Morphology and Performance
Cobalt molybdenum sulfide-type mixed alcohol catalysts were synthesized via calcination of precipitated bulk sulfides and studied with temperature programmed decomposition analysis. Precursors containing aqueous potassium were also considered. Precipitates thermally decomposed in unique events which released ammonia, carbon dioxide, and sulfur. Higher temperature treatments led to more crystalline and less active catalysts in general with ethanol productivity falling from 203 to 97 g (kg cat){sup -1} h{sup -1} when the calcination temperature was increased from 375 to 500 C. The addition of potassium to the precursor led to materials with crystalline potassium sulfides and good catalytic performance. In general, less potassium was required to promote alcohol selectivity when added before calcination. At calcination temperatures above 350 C, segregated cobalt sulfides were observed, suggesting that thermally decomposed sulfide precursors may contain a mixture of molybdenum and cobalt sulfides instead of a dispersed CoMoS type of material. When dimethyl disulfide was fed to the precursor during calcination, crystalline cobalt sulfides were not detected, suggesting an important role of free sulfur during decomposition.
09 BIOMASS FUELS↗
Compositional inhomogeneityand segregation in (K 0.5 Na 0.5 )NbO 3 ceramics
The effects of the calcination temperature of (K 0.5 Na 0.5 )NbO 3 (KNN) powder on the sintering and piezoelectric properties of KNN ceramics have been investigated in this report. KNN powders are synthesized via the solid-state approach. Scanning electron microscopy and X-ray diffraction characterizations indicate that the incomplete reaction at 700 °C and 750 °C calcination results in the compositional inhomogeneity of the K-rich and Na-rich phases while the orthorhombic single phase is obtained after calcination at 900 °C. During the sintering, the presence of the liquid K-rich phase due to the lower melting point has a significant impact on the densification, the abnormal grain growth and the deteriorated piezoelectric properties. From the standpoint of piezoelectric properties, the optimal calcination temperature obtained for KNN ceramics calcined at this temperature is determined to be 800 °C, with piezoelectric constant d 33 =128.3 pC/N, planar electromechanical coupling coefficient k p =32.2%, mechanical quality factor Q m =88, and dielectric loss tan δ=2.1%.
36 MATERIALS SCIENCE↗
Synthesis and characterization of anatase TiO{sub 2} nanotubes with controllable crystal size by a simple MWCNT template method
Highly crystalline phase-pure anatase TiO{sub 2} nanotubes were produced by performing a simple calcinations process in air of the TiO{sub 2} coated MWCNTs composite material prepared by an in situ sol-gel method. A homogeneous thin coating layer of TiO{sub 2} on the surface of MWCNTs is firstly obtained. Calcination in ambient air at appropriate temperatures is performed to transform phase of TiO{sub 2} into anatase and remove MWCNTs simultaneously, resulting in pure anatase TiO{sub 2} nanotubes. Both end tips of the nanotubes are observed to be closed, probably due to covering up MWCNTs with TiO{sub 2} particles. The crystallization of anatase phase was formed upon 350 Degree-Sign C, and MWCNTs are completely oxidized between 500 and 650 Degree-Sign C, leaving anatase TiO{sub 2} nanotubes with an average crystal size increasing from about 8 to 24 nm as the temperature rises. Moreover, the tubular structure was found to collapse after calcinations at 700 Degree-Sign C. - Graphical abstract: TGA analysis and TEM images of the samples after calcinations in air at different temperatures: (a) before calcinations, (b) 350 Degree-Sign C, (c) 500 Degree-Sign C, and (d) 650 Degree-Sign C. Highlights: Black-Right-Pointing-Pointer Highly crystalline and stable phase-pure anatase TiO{sub 2} nanotubes were produced by a simply MWCNT template method. Black-Right-Pointing-Pointer A homogeneous thin coating layer of TiO{sub 2} on the surface of MWCNTs could be obtained. Black-Right-Pointing-Pointer Small crystal size of anatase is formed at lower temperatures and higher temperatures cause significant increase of crystal size from 8 to 24 nm. Black-Right-Pointing-Pointer Convex closed tip structure of TiO{sub 2} nanotubes is formed owing to the good coating of TiO{sub 2}.
36 MATERIALS SCIENCE↗
Synthesis of porous sheet-like Co{sub 3}O{sub 4} microstructure by precipitation method and its potential applications in the thermal decomposition of ammonium perchlorate
Porous sheet-like cobalt oxide (Co{sub 3}O{sub 4}) were successfully synthesized by precipitation method combined with calcination of cobalt hydroxide precursors. The structure, morphology and porosity properties of the products were characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and nitrogen adsorption-desorption measurement. The as-prepared sheet-like microstructures were approximately 2-3 {mu}m in average diameter, and the morphology of the cobalt hydroxide precursors was retained after the calcination process. However, it appeared a large number of uniform pores in the sheets after calcination. In order to calculate the potential catalytic activity, the thermal decomposition of ammonium perchlorate (AP) has been analyzed, in which cobalt oxide played a role of an additive and the porous sheet-like Co{sub 3}O{sub 4} microstructures exhibited high catalytic performance and considerable decrease in the thermal decomposition temperature of AP. Moreover, a formation mechanism for the sheet-like microstructures has been discussed. - Graphical abstract: Porous sheet-like Co{sub 3}O{sub 4} were synthesized by facile precipitation method combined with calcination of {beta}-Co(OH){sub 2} precursors. Thermogravimetric-differential scanning calorimetric analysis indicates potential catalytic activity in the thermal decomposition of ammonium perchlorate. Highlights: Black-Right-Pointing-Pointer Synthesis of sheet-like {beta}-Co(OH){sub 2} precursors by precipitation method. Black-Right-Pointing-Pointer Porous sheet-like Co{sub 3}O{sub 4} were obtained by calcining {beta}-Co(OH){sub 2} precursors. Black-Right-Pointing-Pointer The possible formation mechanism of porous sheet-like Co{sub 3}O{sub 4} has been discussed. Black-Right-Pointing-Pointer Porous sheet-like Co{sub 3}O{sub 4} decrease the thermal decomposition temperature of ammonium perchlorate.
36 MATERIALS SCIENCE↗