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At least 127 records · Page 7
All sourcesNASA NTRSDOE OSTI
DOE OSTI2015

Analysis of slags using laser-induced breakdown spectroscopy

The feasibility of laser-induced breakdown spectroscopy (LIBS) for the analysis of gasification slags was investigated by comparing LIBS results to the results of an ICP-OES analyzer. A small amount of slag sample was placed on a piece of double sided adhesive tape attached to a glass microscope slide and analyzed for Al, Ca, Fe, Si, and V which are major elements found in slags. The partial least squares regression (PLS-R) and univariate simple linear regression (SLR) calibration methods indicated that apart from V (accuracy up to + 20%) the accuracy of analysis varies within 0.35–6.5% for SLR and 0.06–10% for PLS-R. A paired-sample t-test within the 95% confidence level yielded p-values greater than 0.05, meaning no appreciable statistical difference was observed between the univariate SLR with internal standardization and the multivariate PLS-R for most of the analytes. From the results obtained in this work, LIBS response varies depending on the element and the technique used for quantitative analysis. Simultaneous use of the univariate calibration curves with internal standard (intensity ratio) and PLS regression in multi-elemental analysis can help reduce the matrix effect of slags associated to their high variation in concentration. Overall, these results demonstrate the capability of LIBS as an alternative technique for analyzing gasification slags. Estimated limits of detection for Al, Ca, Fe, Si and V were 0.167, 0.78, 0.171, 0.243 and 0.01 wt.%, respectively.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Fiber-Optic Raman Probe for On-line EAF Slag Analysis

Here, in Electric Arc Furnace (EAF) steelmaking, the push for improved efficiency requires accurate analysis of the chemical composition of its slag system to control slag foaming, provide refractory protection, and maintain high furnace iron yield. Therefore, the ability to obtain real-time slag chemistry data would provide a useful tool to improve the control and efficiency of the process. The work reported here aims to assess the structure and chemistry of EAF slags at high temperatures using a portable fiber-optic Raman probe. As a result, the ability to relate Raman spectra peaks to chemistry and structure is demonstrated in experimental result with EAF slags at 1550°C.

47 OTHER INSTRUMENTATION↗
DOE OSTI2026

Evidence for carbon dioxide removal via enhanced rock weathering with steel slag, though not basalt, in a midwestern U.S. field trial

Enhanced weathering is an emergent pathway for permanent atmospheric carbon dioxide removal (CDR). However, despite a dramatic increase in academic and commercial research, there remain relatively few published examples of field evidence demonstrating the effectiveness of enhanced weathering. Here, we present results from a three-year field trial that evaluated steel slag and crushed basalt applied as amendments in a conventional agricultural system in the Midwestern United States. Steel slag applied to initially acidic soil increased porewater pH and alkalinity and increased soil pH and Ca-saturation. Together, changes in porewater chemistry and soil properties provide strong evidence for steel slag weathering and CDR. However, steel slag applied to soils with a neutral initial pH did not generate significant changes in soil or porewater chemistry. In addition, coarse-grained crushed basalt did not generate significant change in any of the soils. Strong acid effects were apparent in all 3 years of monitoring soil porewater chemistry. Overall, our results demonstrate clear evidence of CDR from applying steel slag amendments to acidic cropland soils while also highlighting the difficulty of greenhouse gas reduction accounting from enhanced weathering and the variable outcomes that can occur depending on feedstock and soil type.

Geosciences↗
DOE OSTI2019

Slags as Evidence for Copper Mining above Casaccia, Val Bregaglia (Central Alps)

Slags from the remote Mota Farun locality above Casaccia (Val Bregaglia, Swiss Alps) have been analyzed with scanning electron microscopy, X-ray powder diffraction and microfocus synchrotron X-ray diffraction to determine mineralogical composition and microstructures. Non-magnetic slag samples are largely composed of euhedral and dendritic iron-rich olivine in a glassy matrix. Locally there are zones with globular inclusions rich in bornite ((Cu5Fe)S4) and locally metallic copper. Some regions display dendritic pentlandite ((Fe,Ni)9S8). Magnetic samples are mainly composed of fayalite (Fe2SiO4) and wüstite (FeO), with minor magnetite (Fe3O4). The mineralogical composition indicates that slags were the product of copper smelting. The slag compositions and morphologies are analogous to slags described from the Oberhalbstein (Graubünden, Switzerland) and the Trentino Alps (Italy) which are attributed to metallurgical exploitations of the Late Bronze Age. While the origin of the ore could not be determined, it may be related to ore deposits of chalcopyrite in greenschists and serpentinites in the vicinity, such as Alp Tgavretga (Septimer Pass) and Val Perossa (Val Bregaglia).

58 GEOSCIENCES↗
DOE OSTI2012

Mechanism of Phase Formation in the Batch Mixtures for Slag-Bearing Glass Ceramics - 12207

Slag surrogate was produced from chemicals by heating to 900 deg. C and keeping at this temperature for 1 hr. The product obtained was intermixed with either sodium di-silicate (75 wt.% waste loading) or borax (85 wt.% slag loading). The mixtures were heat-treated within a temperature range of 25 to 1300 deg. C. The products were examined by X-ray diffraction and infrared spectroscopy. The products prepared at temperatures of up to 1000 deg. C contained both phase typical of the source slag and intermediate phases as well as phases typical of the materials melted at 1350 deg. C such as nepheline, britholite, magnetite and matrix vitreous phase. Vitrification process in batch mixtures consisting of slag surrogate and either sodium di-silicate or sodium tetraborate runs through formation of intermediate phases mainly silico-phosphates capable to incorporate Sm as trivalent actinides surrogate. Reactions in the batch mixtures are in the whole completed by ∼1000 deg. C but higher temperatures are required to homogenize the products. If in the borate-based system the mechanism is close to simple dissolution of slag constituents in the low viscous borate melt, then in the silicate-based system the mechanism was found to be much complicated and includes re-crystallization during melting with segregation of newly-formed nepheline type phase. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2013

Gel nanostructure in alkali-activated binders based on slag and fly ash, and effects of accelerated carbonation

Binders formed through alkali-activation of slags and fly ashes, including ‘fly ash geopolymers’, provide appealing properties as binders for low-emissions concrete production. However, the changes in pH and pore solution chemistry induced during accelerated carbonation testing provide unrealistically low predictions of in-service carbonation resistance. The aluminosilicate gel remaining in an alkali-activated slag system after accelerated carbonation is highly polymerised, consistent with a decalcification mechanism, while fly ash-based binders mainly carbonate through precipitation of alkali salts (bicarbonates at elevated CO{sub 2} concentrations, or carbonates under natural exposure) from the pore solution, with little change in the binder gel identifiable by nuclear magnetic resonance spectroscopy. In activated fly ash/slag blends, two distinct gels (C–A–S–H and N–A–S–H) are formed; under accelerated carbonation, the N–A–S–H gel behaves comparably to fly ash-based systems, while the C–A–S–H gel is decalcified similarly to alkali-activated slag. This provides new scope for durability optimisation, and for developing appropriate testing methodologies. -- Highlights: •C-A-S-H gel in alkali-activated slag decalcifies during accelerated carbonation. •Alkali-activated fly ash gel changes much less under CO{sub 2} exposure. •Blended slag-fly ash binder contains two coexisting gel types. •These two gels respond differently to carbonation. •Understanding of carbonation mechanisms is essential in developing test methods.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Sintering and collapse of synthetic coal ash and slag cones as observed through constant heating rate optical dilatometry

Ash agglomeration and slagging are responsible for costly maintenance problems in coal-fired boilers. Boiler design and operation rely on critical ash fusion temperatures defined by geometric criteria that explicitly ignore shrinkage or warping. Reproducibility of ash fusion test (AFT) results is known to be a major problem, given the subjective nature of some criteria used in critical temperature reporting. Decades of faulty predictions based on AFT data underscore the need for an objective measure of the likelihood for agglomeration and slagging as a function of coal ash composition and temperature. Heating microscopes and ash fusibility determinators are AFT instruments that are widely available and readily adapted for optical dilatometry of ash cones through digital image analysis. Optical dilatometry enables the continuous measurement of cone height and face area, and the calculation of changes in cone volume and density as a function of temperature during constant heating. A strong correlation was found between the sintering onset temperatures of two synthetic ash compositions measured through optical dilatometry and their corresponding solidus temperatures predicted through thermophysical modeling. The sintering onset temperatures of synthetic slag cones appears consistent with glass transition temperatures estimated using the Kauzmann-Beaman rule. Cone collapse is highly correlated with softening, hemispherical, and fluid temperatures for ash cones. Rapid changes in solid, liquid, and gas volume fractions near the collapse temperature suggest that a transition from capillary to slurry state may play an important role in triggering collapse. Slag cone collapse is better explained by a decrease in viscosity as a function of temperature in the glass working range. Furthermore, the sintering onset temperature and cone collapse temperature are readily understood through thermophysical modeling based on ash composition and provide two additional critical temperatures in the modeling of coal ash agglomeration and slagging.

01 COAL, LIGNITE, AND PEAT↗
DOE OSTI2020

Controlled evolution of rare earth phosphate in coal ash slag

Coal ash slag as a waste by-product, is generated from commercial processes that include gasification facilities, power plants, and steelmaking industries. Some is recycled into construction materials, insulation fibers, and used as a soil neutralizer, but the majority is still discarded. Coal ash slag exhibit trace amounts of critical materials including rare earth elements (REEs). An economically viable extraction of REEs from the coal ash would lower the production costs, addressing the availability and environmental concerns. In nature, most REEs exist as phosphate such as monazite but its synthetic evolution in coal ash slag has never been reported. In industrial processes, P may originate from coal, additives, and/or refractory liners. REEs may be extracted by first concentrating REEs into phosphates, sulphide, or fluorides [1], or carbonates [2]. In this work, P-enriched coal ash slag bearing REEs was first melted above 1600 °C, then crystallization behaviors in the melt during controlled cooling was studied. REE phosphate coprecipitated with mullite and hematite with mullite being the first crystal to form on cooling. The REEs were rejected from the molten slag, mullite, and hematite, and tended to segregate only to the phosphate phase with REE concentration as high as 58 wt.% in the structure.

Nakano, Jinichiro↗
DOE OSTI2021

Controlled evolution of rare earth phosphate in coal ash slag

Coal ash slag as a waste by-product, is generated from commercial processes that include gasification facilities, power plants, and steelmaking industries. Some is recycled into construction materials, insulation fibers, and used as a soil neutralizer, but the majority is still discarded. Coal ash slag exhibit trace amounts of critical materials including rare earth elements (REEs). An economically viable extraction of REEs from the coal ash would lower the production costs, addressing the availability and environmental concerns. In nature, most REEs exist as phosphate such as monazite but its synthetic evolution in coal ash slag has never been reported. In industrial processes, P may originate from coal, additives, and/or refractory liners. REEs may be extracted by first concentrating REEs into phosphates, sulphide, or fluorides [1], or carbonates [2]. In this work, P-enriched coal ash slag bearing REEs was first melted above 1600 °C, then crystallization behaviors in the melt during controlled cooling was studied. REE phosphate coprecipitated with mullite and hematite with mullite being the first crystal to form on cooling. The REEs were rejected from the molten slag, mullite, and hematite, and tended to segregate only to the phosphate phase with REE concentration as high as 58 wt.% in the structure.

Nakano, Jinichiro↗
DOE OSTI2024

Effect of Si Content in Electrode and SiO2 Additions to the Slag during Electroslag Remelting

Evolution of Si concentration in 316 stainless steel electrodes was observed during a melting campaign consisting of recycling electroslag remelted (ESR) ingots to make new electrodes using vacuum induction melting (VIM). This campaign consisted of iterations of VIM + ESR operations to optimize melting parameters. The effect of Si content on the melt parameters and ingot quality was further evaluated and additions of SiO2 to the slag chemistry were studied using research-scale experiments, x-ray diffraction (XRF), combustion analysis, visual inspections, and computational tools. The Si concentration was found to decrease by approximately 600 ppm following ESR of 150 lb. research-scale electrodes. Eventually, this led to failure of the slag skin and direct ingot/crucible contact. Additions of SiO2 to the slag at levels matching the original calculated Si concentration in the electrode did not eliminate the slag skin failure and the current during steady state increased to maintain a constant melt rate. In this investigation, we propose a mechanism of slag skin failure consisting of local concentration of current density due to absence, or breakage, of the SiO2 layer around the molten metal drop during ESR. This theory was reinforced by additional experiments in which Nb was added to the electrode to change the structure of the oxide layer around the drops.

Jablonski, Paul↗
DOE OSTI2025

CFD modeling and simulation for corrosive wear of refractory in molten slag

The development of high-wear resistant refractories having minimal production costs is facilitated by characterizing the wear mechanisms associated with their corrosive wear. Static cup testing is a commonly used method for comparing the corrosion resistance performance of two or more refractory materials. Although the static cup test conditions are not as severe as dynamic tests, this study shows that the thermal gradient present within the system during heating and cooling stages serves to generate movement of the slag leading to mechanical wear. The thermal gradient within the refractory, and between the slag and the refractory, occurs during the ramp stage of the test and lasts until the soaking stage is reached bringing the system to a thermal equilibrium. Using computational fluid dynamics (CFD) capabilities embedded within ANSYS software, this study modelled and quantified the convection currents within the slag and associated shear stresses generated on the refractory walls due to the thermal gradient. A traditional ladle furnace was employed as a case study to verify the results of the studied CFD model. The corrosion rate of the refractory lining was found to depend on the mass transfer coefficient of the refractory dissolution into the slag, and a velocity term which governs the extent of corrosion at any given location. This velocity term is a function of slag viscosity, as well as the concentration gradient and/or temperature gradient at the triple points. In this study, wall shear stress was used as a reliable proxy for identifying high-velocity regions prone to excessive corrosive wear. Elevated wall shear stress near the slag/air and slag/molten steel interfaces align with observed corrosion grooves, which reflects the intensified corrosive wear at these locations.

Ramteke, Rajat Rajat Durgesh Ramteke [University o↗
DOE OSTI2017

A Structural Study on the Foaming Behavior of CaO-SiO{sub 2}-MO (MO = MgO, FeO, or Al{sub 2}O{sub 3}) Ternary Slag System

The foaming index of the CaO-SiO{sub 2}-MO (MO = MgO, FeO, or Al{sub 2}O{sub 3}) ternary slag system with a fixed CaO/SiO{sub 2} ratio is measured to understand the effect of the ionic structure. At 1773 K (1500 °C), the foaming index of the slag increases with Al{sub 2}O{sub 3} addition and decreases with MgO or FeO addition at a fixed CaO/SiO{sub 2} ratio. It is verified that the previous correlation between the foaming index and the physical properties could also be valid for the CaO-SiO{sub 2}-(MgO or Al{sub 2}O{sub 3}) system. Raman spectroscopy for the CaO/SiO{sub 2} = 1.0 slag is applied to explain the foaming behavior from an ionic structural perspective. From the ionic structural viewpoint, the fractional change in each silicate anion unit is identified by de-convoluted Raman spectra. The Raman spectra indicate that the silicate network structure is polymerized with Al{sub 2}O{sub 3} as an aluminosilicate structure; in contrast, de-polymerization occurs by MgO or FeO addition. Furthermore, the relationship between the silicate structure and the thermodynamic stability function is discussed. Since the ionic structure of the molten slag affects various physical/thermodynamic properties, the foaming behavior could be successfully interpreted from the ionic structural viewpoint.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Rheological Evolution of Ti-Bearing Slag with Different Volume Fractions of TiN

The effect of the volume fraction of TiN (0 to 4.27 vol pct) on the rheological behaviors of Ti-bearing slag, including the viscosity and the constitutive equation, was investigated using a Brookfield rheometer at 1773 K. With the increasing TiN, the viscosity and the shear stress increased substantially, and the slag is converted from Newtonian to non-Newtonian. When the slag samples were dispersed with TiN (1.00 to 4.27 vol pct), the measured viscosities were greater than those estimated by the Einstein–Roscoe equation, and the complex internal structure was suggested to be responsible for the extra enhancement of the viscosity beyond that caused by TiN itself. The viscosity curves of the slag samples containing TiN (1.00 to 4.27 vol pct) were divided into three regions depending on the critical shear rate and the initial shear rate. In the Newtonian region, the apparent volume fraction of TiN was defined and used to develop a semiempirical model based on the Einstein–Roscoe equation to describe the viscosity. In the two non-Newtonian regions, the shear rate, the yield stress, and the viscosity differences between the non-Newtonians regions and the Newtonian regions were applied in developing the viscosity models.

36 MATERIALS SCIENCE↗
DOE OSTI2018

In Situ Observation of Calcium Aluminate Inclusions Dissolution into Steelmaking Slag

The dissolution rate of calcium aluminate inclusions in CaO-SiO{sub 2}-Al{sub 2}O{sub 3} slags has been studied using confocal scanning laser microscopy (CSLM) at elevated temperatures: 1773 K, 1823 K, and 1873 K (1500 °C, 1550 °C, and 1600 °C). The inclusion particles used in this experimental work were produced in our laboratory and their production technique is explained in detail. Even though the particles had irregular shapes, there was no rotation observed. Further, the total dissolution time decreased with increasing temperature and decreasing SiO{sub 2} content in the slag. The rate limiting steps are discussed in terms of shrinking core models and diffusion into a stagnant fluid model. It is shown that the rate limiting step for dissolution is mass transfer in the slag at 1823 K and 1873 K (1550 °C and 1600 °C). Further investigations are required to determine the dissolution mechanism at 1773 K (1500 °C). The calculated diffusion coefficients were inversely proportional to the slag viscosity and the obtained values for the systems studied ranged between 5.64 × 10{sup −12} and 5.8 × 10{sup −10} m{sup 2}/s.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Prediction and Measurement of the Kinetics of Isothermal Crystallization and Devitrification of Mold Powder Slags

The rate and extent of formation of crystalline phases in the slag film that develops between the mold and the strand in steel continuous casting determine heat transfer and lubrication between them and therefore play crucial roles in shell integrity. In this work, a commercial mold powder for casting medium carbon (MC) thin steel slabs is selected for carrying out detailed comparisons between predicted and experimental results of the rates of isothermal crystallization and devitrification of liquid and glassy slag, respectively. Predictions are obtained with a kinetic model that combines the induction period (of Šimon and Kolman) and the Kissinger methods to evaluate time–temperature–transformation (TTT) diagrams for the devitrification and crystallization reactions associated with the peaks appearing in non-isothermal thermo-analysis traces. To obtain experimental validation of the diagram, a high-temperature confocal laser scanning microscope (HT-CLSM) is used to rapidly heat or cool a sample, ~ 140 mg, of glassy powder or liquid slag, respectively, to selected isothermal conditions, where it is held for a prescribed length of time before quenching. Identification and quantification of the phases present in the quenched samples are done by a quantitative X-ray powder diffraction analysis (QXRPDA) method that uses a PONKCS (partial or not known crystal structure) procedure based on Le Bail and Rietveld strategies for refinement of diffraction patterns. The many experimental results indicate that the predicted TTT diagrams for devitrification and crystallization of the mold slag give a good estimation of the rate of the transformations that take place at different temperatures and reveal the differences in the reactions that occur along both paths.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Thermodynamic Study on MgO Solubility in High-Alumina-Content Slag System

In the current study, the MgO solubility in molten slag was measured to clarify the effect of basicity and Al{sub 2}O{sub 3} content on the MgO solubility equilibrating with the spinel solid phase in the CaO-SiO{sub 2}-Al{sub 2}O{sub 3} system. The MgO solubility decreased with the increasing basicity of the slag. However, the MgO solubility in the spinel equilibrium region exhibited different dependence when compared with the basicity dependence in the MgO equilibrium region. The aforementioned experimental results were quantitatively analyzed using magic-angle spinning (MAS) {sup 27}Al nuclear magnetic resonance (NMR) spectroscopy, in which the fraction of Al ions in the slag of spinel equilibrium region was changed to 4, 5, and 6. In addition, the analysis of the degree of Al avoidance modeling indicated that the change in bridging oxygen (BO) linkage species (distinguished into Al-O-Al, Si-O-Si, and Al-O-Si) was based on the Al/Si ratio change. The aforementioned change in BO linkage species led to a change in the MgO solubility with the stability of the alumina. Thus, the spinel equilibrium dissolution mechanism is discussed in detail in terms of the thermodynamic and structural influence in molten slag.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Influence of Aluminum-Carbon Composite Pellets on FeO Reduction and Iron Recovery from Electric Arc Furnace Slag

We investigated the effect of Al-C composite pellets (ACCP) on the reduction behavior of FeO in electric arc furnace (EAF) slag and the iron recovery at different n{sub Al}/(n{sub Al} + n{sub C}) at 1823 K (1550 °C). A carbothermic reaction was the dominant process at n{sub Al}/(n{sub Al} + n{sub C}) < 0.4, whereas aluminothermic reduction was the major process at n{sub Al}/(n{sub Al} + n{sub C}) > 0.6; these observations are based on the final content of FeO and Al{sub 2}O{sub 3} in the molten slag. The aluminum and carbon present in the ACCP competitively affected the reaction stoichiometry (i.e., the material balance) between the production of CO + Al{sub 2}O{sub 3} and the consumption of FeO. Iron recovery increased up to a yield of approx. 90 pct as the n{sub Al}/(n{sub Al} + n{sub C}) ratio increased. Because Al in the ACCP readily reacts to reduce FeO in the molten slag, iron recovery is proportional to the n{sub Al}/(n{sub Al} + n{sub C}) ratio. The precipitation of solid compounds in the slag phase, such as monoxide ([Mg,Fe]·O) and spinel (MgO·Al{sub 2}O{sub 3}), occurred during FeO reduction; this was experimentally confirmed as well as by thermochemical computation. Furthermore, we proposed a schematic reaction mechanism in the present study.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Kinetics and Mechanisms of Dolime Dissolution in Steelmaking Slag

The kinetics of dolime dissolution containing 20 and 50 pct of magnesium oxide in steelmaking slags has been studied in a high-temperature experiment. The dissolution tests were carried out under static conditions at temperatures of between 1573 K and 1873 K (1300 °C to 1600 °C). Cylindrical samples of dolime were introduced into pre-melted slag at predetermined time intervals. The changes in mass and geometrical parameters of the samples, as well as CaO and MgO concentrations in the melt, were determined to calculate mass transfer and diffusion coefficients. The results revealed that the rate-limiting step in the process of dolime dissolution is diffusion. The increase in MgO content in the initial sample caused a drop in dolime dissolution rate and diffusion coefficients. The prediction of MgO solubility in steel slag, as well as the effect of slag basicity, was carried out using the thermodynamic software FactSage 7.1. In addition, the activation energy of diffusion has been calculated using the dependence of the logarithm of diffusion coefficients on the inverse temperature.

36 MATERIALS SCIENCE↗