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At least 19 records

Influence of baking method and baking temperature on the optical properties of ZnO thin films

In this work, sol-gel spin coating technique was utilised to coat ZnO thin films on glass substrates. During the intermediate 3 minutes baking process, either hotplate or convection oven was employed to bake the samples. The temperature for the baking process was varied from 150°C to 300°C for both instruments. Avantes Optical Spectrophotometer was used to characterise the optical property. The optical transmittances of hotplate-baked and oven-baked samples showed different trends with increasing baking temperatures, ranging from below 50% transmittance to over 90% transmittance in the visible range of wavelength. The difference in baking mechanisms using hotplate and convection oven will be discussed in this paper.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Improving the Performance of Mid-T Baked Niobium Cavities through Post-Bake Surface Treatment

he Medium temperature (mid-T) baking of niobium superconducting radio-frequency cavities at 300 350 C in a vacuum furnace is known to enhance the quality factor (Q₀). However, despite this improvement, cavities treated with this process often exhibit premature quench at relatively low accelerating fields. This limitation is suspected to arise from the formation of surface contaminants, such as niobium carbides, during the furnace bake at 350 C for 3 h. To investigate the influence of potential surface contamination, this study applied an ultralight chemical removal to 1.3 GHz and 650 MHz single-cell cavities that had undergone medium-temperature baking. The removal of the top RF surface layer led to a notable improvement in the quench field and Q₀, indicating a beneficial effect of eliminating possible surface residues introduced during the bake.

Chouhan, Vijay [Fermilab]↗

Improving the performance of mid-T baked niobium cavities through post-bake surface treatment

The Medium temperature (mid-T) baking of niobium superconducting radio-frequency cavities at 300 350 C in a vacuum furnace is known to enhance the quality factor (Q₀). However, despite this improvement, cavities treated with this process often exhibit premature quench at relatively low accelerating fields. This limitation is suspected to arise from the formation of surface contaminants, such as niobium carbides, during the furnace bake at 350 C for 3 h. To investigate the influence of potential surface contamination, this study applied an ultralight chemical removal to 1.3 GHz and 650 MHz single-cell cavities that had undergone medium-temperature baking. The removal of the top RF surface layer led to a notable improvement in the quench field and Q₀, indicating a beneficial effect of eliminating possible surface residues introduced during the bake.

Chouhan, V. [Fermilab] (ORCID:0000000282004931)↗

Strong Meissner screening change in superconducting radio frequency cavities due to mild baking

We investigate “hot” regions with anomalous high field dissipation in bulk niobium superconducting radio frequency cavities for particle accelerators by using low energy muon spin rotation (LE-μSR) on corresponding cavity cutouts. We demonstrate that superconducting properties at the hot region are well described by the non-local Pippard/BCS model for niobium in the clean limit with a London penetration depth λ{sub L}=23±2 nm. In contrast, a cutout sample from the 120 ∘C baked cavity shows a much larger λ>100 nm and a depth dependent mean free path, likely due to gradient in vacancy concentration. We suggest that these vacancies can efficiently trap hydrogen and hence prevent the formation of hydrides responsible for rf losses in hot regions.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

AN ACID BAKING APPROACH TO ENHANCE RARE EARTH ELEMENT RECOVERY FROM BITUMINOUS COAL SOURCES

Rare earth elements (REE) are a group of 17 elements typically classified as light and heavy rare earth elements, which play a crucial role in developing the latest technologies for energy, defense, and medical sectors. Even though REEs have been found in more than 200 minerals, only bastnaesite, monazite and xenotime are commercially exploited for REE extraction. However, the recent exponential increase in REE demand has spurred countries such as the United States into research for the extraction of REEs from secondary sources such as coal, acid mine drainage, and coal ash. Several coal sources (e.g., Fire Clay seam coal) across the United States have been identified to contain elevated concentrations of rare earth elements (>600 ppm), and various researchers have investigated the feasibility of both physical and hydrometallurgical extraction techniques for rare earth concentration and subsequent extraction. However, both physical and direct leaching were concluded to be inefficient for RE beneficiation and extraction due to low recoveries. Alternatively, thermal treatment provides promising means for RE recovery from bituminous coal sources. The positive impact of thermal treatment/calcination was established to be due to the decarbonization and dehydroxylation of the clays, which released entrapped rare earth elements within the dominant minerals and converted them into an acid-soluble form. Nonetheless, the improvement in recovery was limited to the light REEs (LREEs) with an insignificant increase in the heavy REEs (HREE). It was demonstrated that the light and heavy REEs in the material were associated with difficult-to-leach minerals such as monazite, xenotime, and zircon, which were not decomposed by simple calcination due to their high thermal stability. Hence, roasting in the presence of chemicals was necessary to ensure the decomposition of those REE-containing minerals. As such, this study was focused on the acid baking treatment of bituminous coals with an aim to enhance REE recovery, especially HREEs. Based on the presence of REE minerals like monazite and xenotime, three pre-leach treatment methods, i.e., 1) roasting, 2) direct acid baking, and 3) acid baking after roasting were investigated. Roasting tests at 600 ⁰C revealed that the recovery of light REEs (LREEs) was enhanced while the recovery of HREEs remained relatively unaffected. LREE and HREE recovery values of 38.3% and 21.3%, respectively, were achieved using a 50 g/L sulfuric acid solution at 5% solid concentration and a solution temperature of 75 ⁰C for 2 hours. Comparatively, direct acid baking at 250 °C provided substantial increased LREE and HREE recovery values to approximately 49.4% and 53.0%, respectively, using an equivalent acid dosage. Recoveries were maximized to 77.0% and 79.6% for LREE and HREE, respectively, by roasting followed by acid baking. Similar results were obtained from the treatment of a second bituminous coal source. Due to strong correlations between REE and Al recovery values, tests were performed on kaolinite and illite, which were prominent clay minerals within the source coals. These experiments revealed that the REE recovery improvements were likely a result of dehydroxylation of clays and subsequent release and decomposition of REE-bearing minerals such as monazite, xenotime and zircon. Subsequently, a parametric study was conducted to identify the impact of acid baking parameters on rare earth element recovery. The factors investigated using a three-level statistical experimental program were acid baking time, acid solution concentration, baking temperature, and acid solution-to-solids ratio which were found to significantly impact REE and contaminant element (Al, Fe, and Ca) recovery. An increase in baking temperature up to around 250 ⁰C improved the light and heavy REE recovery values by more than 50 absolute percentage points relative to performances achieved when direct leaching. As aforementioned, acid baking was needed to both decompose the clay minerals and liberate the REE minerals, which allowed access for the acid to solubilize the REEs. Acid concentration of the solution used for acid baking was studied as a means of minimizing the amount of acid needed to achieve a target REE recovery. However, thermo-gravimetric and differential scanning calorimetry analysis (TGA-DSC) of sulfuric acid under oxidizing atmosphere revealed that the addition of water decreased the evaporation temperature, which explains the lower REE recovery values obtained when using acid concentrations less than 100%. Using pure sulfuric acid at an acid-to-solid ratio of 0.8:1 resulted in recovery values of around 70% for both LREEs and HREEs. The decomposition reaction time was relatively quick with 65% of the TREEs recovered within the first 10 minutes. Following the identification of optimum operating conditions through the parametric study, a systematic leaching study was carried out to examine the impact of leaching parameters, such as solid-to-liquid (S/L) ratio, temperature, and time, on REE recovery using acid baking conditions of 1:1 acid to solids ratio at 250 °C for 30 minutes. The solid-to-liquid ratio was varied from 1-20% by weight at 25 °C, 50 °C, and 75 °C solution temperatures. The results indicated that reaction time and solution temperature considerably impacted the recovery of heavy and light REEs. Interestingly, LREE recovery reduced from 68% at 5% S/L to 58% at 20%S/L, whereas HREE recovery of 78% remained unaffected. The decrease in the LREE recovery was determined to be due to La and Ce precipitation, likely through isomorphic substitution with calcium in gypsum. The kinetic data indicated that 67% LREE and 77% HREE recovery could be obtained within the first 15 minutes of the reaction, suggesting fast reaction kinetics. Furthermore, raising the solution temperature from 25 °C to 75 °C increased the LREE and HREE recovery from 60% and 32% to 67% and 79%, respectively. The kinetic modeling results demonstrated that the rate-limiting step in the LREE dissolution was diffusion and chemical reaction, whereas the HREE extraction was controlled by only chemical reaction. The leaching study concluded that using 20% S/L at 75 °C for 15 minutes maximized LREE and HREE recovery. The lab-scale precipitation study showed that Fe and Al in solution could be removed at pH 4.5 followed by REE precipitation at pH 6.0 using 6 mol/L NaOH. Finally, the bench-scale data was used to develop a process flowsheet for REE recovery from low-grade bituminous coal sources using acid baking. Finally, based on the proposed flowsheet, a concentrated RE-cake obtained through selective precipitation at pH 6.5 was re-leached using HCl at pH 1.5. The resultant leachate was used to identify the impact of various operating parameters on REE recovery and purity with an aim to maximize REE precipitation efficiency while minimizing the oxalic acid dosage. The operating parameters for this investigation were oxalic acid dosage, iron (III) contamination, solution pH and temperature. The resultant model suggested that oxalic acid dosage and reaction pH are the most significant factors for the REE precipitation efficiency, followed by the interaction of oxalic dosage and Fe concentration. Test results indicated that increasing the oxalic acid concentration from 0g/L to 80g/L improved the REE precipitation efficiency from approximately 4.2% to 95.0%. Furthermore, raising the solution pH from 0.5 to 2.5 considerably enhanced the precipitation efficiency from 0.0% to 98.9%. A solution temperature elevation decreased REE recovery, which indicated an exothermic reaction between REEs and oxalate anions. Finally, a high level of Fe contamination adversely impacted REE precipitation efficiency. The speciation analysis revealed that the dominant iron species in the solution system were Fe-(C₂O₄)₃³⁻, Fe-(C₂O₄)²⁻, and Fe-(C₂O₄)⁺, which consumed the majority of the oxalate anions

rare earth elements, acid baking, high-temperature↗

Parametric study of an acid baking process for rare earth element recovery from a bituminous-coal source

Acid baking treatment is widely used to extract rare earth elements (REEs) from refractory rare earth bearing minerals such as monazite and xenotime. Since these REE minerals have been identified in coal-based sources, a parametric study was conducted to evaluate the impact and optimize the parametric values associated with the acid-baking process when treating a bituminous coal source. The parameters studied using a three-level statistical experimental program were acid baking time, acid solution concentration, baking temperature, and acid solution-to-solids ratio and each were found to significantly impact REE and contaminant element recovery. An increase in baking temperature up to around 250°C improved the light and heavy REE recovery values by more than 50 absolute percentage points relative to performances achieved when direct leaching. Acid baking was needed to dehydroxylate the clays and liberate the REE minerals, which allowed access for the acid to solubilize the REEs. Acid concentration of the solution used for acid baking was studied as a means of minimizing the amount of acid needed to achieve a target REE recovery. However, thermo-gravimetric and differential scanning calorimetry analysis (TGA-DSC) of sulfuric acid under oxidizing atmosphere revealed that the addition of water decreased the evaporation temperature, which explains the lower REE recovery values obtained when using lower acid concentrations. Using pure sulfuric acid at an acid-to-solid ratio of 0.8:1 resulted in recovery values of around 70% for both LREEs and HREEs. The decomposition reaction time was relatively quick with 65% of the TREEs recovered within the first 10 minutes. Water leaching experiments performed on the acid-baked products under a temperature of 25°C instead of 75°C revealed an increase in REE recovery by 10 absolute percentage points, which was likely due to the high solubility of REE-sulfates at room temperatures.

01 COAL, LIGNITE, AND PEAT↗

In Situ Monitoring of Pit Gas Composition During Baking of Anodes for Aluminum Electrolysis

Carbon anodes, which are consumed in aluminum electrolysis, are fabricated in separate anode plants where coke and pitch are mixed and vibrocompacted to green anode blocks before being baked in anode baking furnaces. The chemical environment inside an anode baking furnace is found to play an important role in the degradation of the furnace refractory lining. In this work, the pit gas composition was recorded during anode baking by a Fourier transformed infrared spectroscopy (FTIR) spectrometer and a gas chromatograph. The temperature dependence of the concentration of gas species during baking was obtained based on three measurement campaigns. The concentrations of CO and CO{sub 2} were found to be dependent on temperature, where the concentration of CO peaked around the maximum firing temperature. In addition to varying concentrations of CH{sub 4} and HF, water was found in large amounts in the first part of the baking cycle. The water originates to some extent from the cooling of the green anodes after vibrocompaction and is potentially important with respect to the chemical stability of the refractory lining. The variations in pit gas composition are related to operational parameters and are discussed in relation to refractory degradation phenomena.

36 MATERIALS SCIENCE↗

Mechanisms of paint bake response in resistance spot-welded first and third generation AHSS

Implementation of 3rd generation advanced high strength steels (3GAHSS) in automotive structures requires careful consideration of joining process implications. Due to the presence of increased carbon equivalent in 3GAHSS such as 980 HF relative to commonly-applied 1st generation AHSS such as 980 DP, the resultant properties of the weld nugget and heat affected zones in resistance spot welded must be engineered to provide consistent and acceptable performance, specifically in cross-tension loading mode. Although the as-welded cross-tension strength (CTS) of 980 HF is less than 980 DP, there is a significant improvement of the CTS after paint baking in 980 HF welds. 980 DP steel welds do not exhibit such marked improvement upon baking. The mechanism of the strong and beneficial effect of paint baking on 980 HF in comparison to 980 DP is discussed in light of its effect on residual stress distributions and microstructures. Although residual stress (strain) reduction is observed via synchrotron x-ray diffraction for all tested steels, this effect is demonstrated as secondary to the performance restoration of the weld joint in cross tension. High-resolution electron channeling contrast imaging (ECCI) micrographs reveal that paint baking affects a more beneficial degree of martensite tempering in 980 HF as compared to 980 DP. The martensite tempering is also evidenced by both a reduction in nano-hardness of critical microstructural features and re-emergence of ductile fracture behavior following the paint baking process. The tempering of martensite is concluded to be the dominant mechanism in improving cross tension strength of 3GAHSS welds following paint baking.

36 MATERIALS SCIENCE↗

A New Perspective of Post-Weld Baking Effect on Al-Steel Resistance Spot Weld Properties through Machine Learning and Finite Element Modeling

The root cause of post-weld baking on the mechanical performance of Al-steel dissimilar resistance spot welds (RSWs) has been determined by machine learning (ML) and finite element modeling (FEM) in this study. A deep neural network (DNN) model was constructed to associate the spot weld performance with the joint attributes, stacking materials, and other conditions, using a comprehensive experimental dataset. The DNN model positively identified that the post-weld baking reduces the joint performance, and the extent of degradation depends on the thickness of stacking materials. A three-dimensional finite element (FE) model was then used to investigate the root cause and the mechanism of the baking effect. It revealed that the formation of high thermal stresses during baking, from the mismatch of thermal expansion between steel and Al alloy, causes damage and cracking of the brittle intermetallic compound (IMC) formed at the interface of the weld nugget during welding. This in turn reduces the joint performance by promoting undesirable interfacial fracture when the welds were subjected to externally applied loads. The FEM model further revealed that increase in structural stiffness, because of increase in steel sheet thickness, reduces the thermal stresses at the interface caused by the thermal expansion mismatch and consequently lessens the detrimental effect of post-weld baking on the joint performance.

36 MATERIALS SCIENCE↗

Understanding Surface Contamination Effects in Mid-T Baked Cavities

Medium-temperature baking is applied to niobium SRF cavities to enhance their quality factor. However, mid-T baking performed in the 300-350 °C range may lead to the formation of surface carbides, which can prevent the cavities from exhibiting the full benefit of mid-T baking. To investigate the effect of potential surface contaminants, the top RF layer of mid-T-baked cavities was removed using an ultralight electropolishing process. The performance of the mid-T baked cavities was significantly improved after applying this ultralight EP. This presentation summarizes the latest results on this study.

Chouhan, Vijay [Fermilab]↗

An acid baking approach to enhance heavy rare earth recovery from bituminous coal-based sources

The recovery of rare earth elements (REEs) from secondary resources, particularly coal-based materials, has recently received attention due to supply and demand imbalance. Research reported to date indicates that a high REE recovery can be realized when treating bituminous coal sources using strong acid solutions of approximately100 g/L or higher. This study introduces an approach to enhance the total rare earth recovery (TREE), especially for heavy rare earth elements (HREEs), from these coal sources at significantly lower acid concentrations. Based on the presence of REE minerals like monazite and xenotime, a detailed investigation was undertaken to quantify three pre-leach treatment methods, i.e., 1) roasting, 2) direct acid baking, and 3) acid baking after roasting. Roasting tests at 600°C revealed that the recovery of light REEs (LREEs) was enhanced while the recovery of HREEs remained relatively unaffected. LREE and HREE recovery values of 38.3% and 21.3%, respectively, were achieved using a 50 g/L (0.5 M) sulfuric acid solution at 5% solid concentration and a solution temperature of 75°C for 2 h. Comparatively, direct acid baking at 250°C provided substantial increases in LREE and HREE recovery values to approximately 49.4% and 53.0%, respectively, using an equivalent acid dosage. Recoveries were maximized to 77.0% and 79.6% for LREE and HREE, respectively, by roasting followed by acid baking. Similar results were obtained from the treatment of a second bituminous coal source. Due to strong correlations between REE and Al recovery values, tests were performed on kaolinite and illite, which were prominent clay minerals within the source coals. In conclusion, these experiments revealed that the REE recovery improvements were likely a result of dehydroxylation of clays and subsequent release and decomposition of REE-bearing minerals such as monazite, xenotime and zircon.

42 ENGINEERING↗

TMAP modeling of D release from baked multi-layer Be–D co-deposits

Single-layer Beryllium–Deuterium (Be–D) co-deposits were analyzed using Thermal Desorption mass Spectrometry (TDS) as outlined in the companion paper. This work details the TMAP modeling and the analysis of selected samples that received double-layer (DL) coatings to study co-deposit thickness and prior bake effects. Here, TDS data were simulated with detrap energies 0.8, 0.9, and 1.0 eV. In DLs formed at 393 K, modeling revealed that under-layers baked at 623 K for either 2 or 20 h had little pumping effect on over-layers, suggesting empty trap removal during bake. Extrapolated to ITER, data and analysis suggest less impact on the ongoing ITER bake efficiency than previously predicted.

36 MATERIALS SCIENCE↗

Insight to the Duration of 120 °C Baking on the Performance of SRF Niobium Cavities

Low-temperature baking at 100 °C - 140 °C in ultra-high vacuum for several hours is the final cavity processing technique to achieve the highest accelerating gradient cavity by eliminating the high field Q-slope, typically on cavities made of high purity fine grain niobium and subjected to electropolishing. The temperature and duration of baking control the onset of the high field Q-slope and overall quality factor over the baseline measurements. The increase in quality factor is generally related to the reduction in the temperature-dependent surface resistance, which refers to BCS surface resistance due to the reduction in the electronic mean free path and elimination of high field Q-slope is still being actively investigated. Here, we present the results of a series of measurements on 1.3 GHz TESLA shape single-cell cavities with successive low-temperature baking at 120 °C up to 96 hours. The rf loss related to the trapping of residual magnetic field refer to flux trapping sensitivity was measured with respect to the duration of 120 °C bake.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Effect of duration of 120 oC baking on the performance on superconducting radio frequency niobium cavities

Over the last decade much attention was given in increasing the quality factor of superconducting radio frequency (SRF) cavities by impurity doping. Prior to the era of doping, the final cavity processing technique to achieve the high accelerating gradient includes the ?in situ? low temperature baking of SRF cavities at temperature ~ 120 oC for several hours. Here, we present the results of a series of measurements on 1.3 GHz TESLA shape single-cell cavities with successive low temperature baking at 120 oC up to 96 hours. The experimental data were analyzed with available theory of superconductivity to elucidate the effect of the duration of low temperature baking on the superconducting properties of cavity materials as well as the rf performance. In addition, the rf loss related to the trapping of residual magnetic field refereed as flux trapping sensitivity was measured with respect to the duration of 120 oC bake.

Khanal, B. D.↗

Mitigation of distortion of Al/steel part under simulated paint baking condition: Experiment and numerical model studies

Multi-material joining of lightweight structures is essential to reduce vehicle weight for more energy savings and less greenhouse gas emission. However, mismatch of thermal expansion coefficient for dissimilar materials during the paint baking process can induce part distortion and joint failure for adhesive bonding. Here, in the present work, a thermomechanical model based on contact mechanics and large deformation theory was developed for dissimilar high-strength Al alloy and steel components to study the distortion mechanism and influential factors of the residual gap. The established model was used to optimize joint conditions, such as pitch distance and part geometry. When a weld pitch is shorter than 100 mm, the maximum gap between Al and steel part can be greatly reduced to 0.1 mm, and the local stress and plastic strain around the joint during the oven heating and cooling cycle are also substantially reduced compared with the long pitch case (900 mm). The numerical modeling results revealed that a comparable bending stiffness ratio between the steel and Al cross sections is critical to the minimization of gap and distortion under paint baking condition. Digital image correlation technique was used to measure the overall part distortion and local strain distribution that were used to validate the model prediction. Weld bonding (adhesive bonding with friction bit joining) process was successfully employed to join Al to steel component without gap opening in adhesive after the paint baking and cooling.

36 MATERIALS SCIENCE↗

Preliminary observation on the effect of baking soda volume on controlling odour from discarded organic waste

Highlights: • Approximately 50 g baking soda reduced odour concentration by 70%. • Reducing volatile acid concentration reduces odour concentration. • Ammonia has less effect on odour concentration. - Abstract: Food wastes with high moisture and organic matter content are likely to emit odours as a result of the decomposition process. The management of odour from decomposing wastes is needed to sustain the interest of residents and local councils in the source separation of kitchen wastes. This study investigated the potential of baking soda (at 50 g, 75 g and 100 g per kg food waste) to control odour from seven days stored food waste. It was found that 50 g of baking soda, spread at the bottom of 8 l food wastes bin, can reduce the odour by about 70%. A higher amount (above 100 g) is not advised as a pH higher than 9.0 may be induced leading to the volatilization of odorous ammonia. This research finding is expected to benefit the waste management sector, food processing industries as well as the local authorities where malodour from waste storage is a pressing issue.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Evidence of incomplete annealing at 800 °C and the effects of 120 °C baking on the crystal orientation and the surface superconducting properties of cold-worked and chemically polished Nb

High-purity niobium rods were cold-worked by wire-drawing, followed by various combinations of chemical polishing and high-vacuum baking at 120 °C or annealing at 800 °C in order to better understand changes to the surface superconducting properties resulting from typical superconducting radio-frequency cavity processing. AC susceptibility measurements revealed an enhanced upper transition T c at ~ 9.3–9.4 K in all samples that was stable through all annealing steps, a value significantly above the accepted T c of 9.23 K for pure annealed niobium. Corresponding elevations were seen in the critical fields, the ratio of the surface critical field H c3 to the bulk upper critical field H c2 rising to 2.3, well above the Ginzburg–Landau value of 1.695. Orientation imaging revealed an extensive dislocation rich sub-grain structure in the as-drawn rods, a small reduction of the surface strain after baking at 120 °C, and a substantial but incomplete recrystallization near the surface after annealing at 800 °C. We interpret these changes in surface superconducting and structural properties to extensive changes in the near-surface interstitial contamination produced by baking and annealing and to synergistic interactions between H and surface O introduced during electropolishing and buffered chemical polishing.

36 MATERIALS SCIENCE↗

Performance enhancement of medium temperature baked niobium SRF cavity by surface contamination removal

Medium temperature baking (300- 350 °C) enhances the quality factor of niobium superconducting radio frequency cavities. However, surface contamination introduced during vacuum furnace baking limits the quench field and may also degrade the quality factor of the cavity. To investigate this effect, a 1.3 GHz single-cell Nb cavity underwent mid-T baking, followed by a chemical treatment to remove the surface contaminants. Post-treatment measurements revealed a significant improvement in both the quality factor and the quench field.

Chouhan, Vijay [Fermilab] (ORCID:0000000282004931)↗