Processing Temperature Research Articles

DELIGNIFICATION OF OIL PALM EMPTY FRUIT BUNCHES USING DEEP EUTECTIC SOLVENT IN PRESSURIZED REACTOR

Although lignin from oil palm empty fruit bunches (OPEFB) is a sustainable bioresource with several value-added uses, it is still difficult to extract lignin from lignocellulosic biomass economically. Lignin fractions are required for high-value applications and subsequently increase the feasibility of lignocellulosic biorefineries. Besides, the remaining cellulose could be further valorized into various chemical products. In this study, the delignification efficiency of OPEFB under inert and pressurized conditions has been studied as an effective pretreatment method for OPEFB. The optimal conditions of the high-pressure reactor to remove lignin from OPEFB were determined to be 80 °C at 30 bars with the presence of deep eutectic solvents (DES). It was identified that pressure affects the removal of lignin with the least amount of structural breakdown and the digestibility of cellulose. The effective removal of lignin from the OPEFB was established under mild conditions employing an inert nitrogen gas pressurized system. This work selectively removes lignin from the OPEFB of palm oil biomass plants using DES under mild extraction conditions. Solid residues were characterized by using FTIR, SEM, TGA, and XRD to investigate fractions under various reaction conditions, such as removal temperature, time, and pressure. The thermal stability of lignin was determined by TGA. In this study, 36.68% of lignin was removed under optimum pressure conditions at the lowest process temperature of 80 °C to determine how these factors influence the efficiency of lignin extraction in a high-pressure reactor.

Mobilities of volatiles (H, F and C) in apatite at high temperatures

Apatite serves as a notable host for diverse volatiles, but experimental data concerning the mobilities of volatiles out of its lattice remains scarce. Despite several investigations elucidating the diffusivities of F, Cl, and OH, their interplay mechanism remains poorly understood. Herein, to unveil the mobilities of hydrogen, fluorine, and carbon out of the apatite lattice and their intricate interaction mechanisms during high temperature processes, we carry out annealing experiments at 900, 1000, and 1100 °C on two apatite samples with distinct fluorine contents. Our findings indicate that along the c-axis, hydrogen diffusion coefficients surpass those of fluorine by 2–3 orders of magnitude, with lower activation energies observed. Hydrogen diffusion shows strong anisotropy, with lager diffusivities and lower activation energies along the c-axis than the a-axis. For both hydrogen and fluorine, the Durango apatite shows smaller diffusivities along the c-axis than the Imilchil apatite. Contrarily, carbon diffusion is absent in both samples at these temperatures. These differences in diffusivity may suggest that hydrogen diffuses as OH− along the a-axis and as H+ along the c-axis, while fluorine diffusion relies on hydrogen diffusion along the c-axis. Based on these new data, the capacity of apatite to record volatiles can be evaluated. All volatiles, including hydrogen, is likely preserved within the core of apatite during thermal events from several days to years, such as rapid volcanic eruptions. However, for prolonged thermal events lasting hundreds of millions of years, apatite preserves volatiles for F, Cl and C, but not hydrogen.

Study on Strain Hardening and Cryogenic Toughness of Marine 10Ni5CrMoV Steel during Tempering

The tempering process is applied in marine 10Ni5CrMoV steel to study microstructure, and mechanical properties by multi‐scale characterizations, strain hardening behavior, and cryogenic toughening mechanism are further investigated. As the tempering temperature increases from 590 to 630 °C, the dislocation density decreases by up to 25% and the austenite volume fraction decreases by up to 35%. Additionally, the morphology of austenite changes from strip to bulk, which weakened the pinning effect on the laths, leading to a coarsened martensite and an increase in the equivalent grain size. Based on the modified Crussard–Jaoul analysis, the specimens at different tempering temperatures exhibit a single‐stage strain hardening behavior during plastic deformation. The increase in strength is attributed to the continuous transformation‐induced plasticity effect and the increasing dislocation density. Furthermore, high austenite volume fraction and the proportion of grain boundary misorientation above 45° promote the release of stress concentration and hinder the propagation of cracks. This results in an increase in the ductile–brittle transition temperature (DBTT) of the specimens from −105 to −135 °C. At a tempering temperature of 610 °C, the specimen demonstrates an outstanding balance between yield strength (868 MPa) and cryogenic toughness (DBTT of −135 °C).

Electrochemical Conversion of CO2 to Fuels and Useful Chemicals over Metal Supported Solid Oxide Electrolyzers

Electrochemical conversion of CO2 and H2O to fuels and chemicals provides a promising approach to simultaneously mitigate greenhouse emission and store surplus energy, which reduces electricity network variation due to increased intermittent renewable energy (such as solar and wind) utilization. Metal supported solid oxide electrolyzers (MS-SOEs) developed at Lawrence Berkeley National Laboratory provide advantages of rapid start-up, mechanical ruggedness, redox tolerance, dynamic operation, and low-cost materials. A relatively high operating temperature range of 600 to 750°C promotes energy efficiency and allows utilization of thermal energy such as steam.In this work, efficient and stable catalysts developed at the University of South Carolina have been infiltrated in the symmetrical and porous MS-SOE architecture. The phase purity has been analyzed by X-day diffraction. The morphologies of these infiltrated and posttest catalysts have been examined by scanning electron microscopy. Optimization of cell structure, processing temperature, cell voltage, and catalyst infiltration cycles for better cell performance will be presented. The stability of MS-SOEs has been evaluated during continuous operation for >200 hours. The cell degradation mechanisms revealed by electrochemical impedance spectroscopy and high-resolution scanning electron microscopy techniques will be presented.In addition to pure CO2 electrochemical conversion, effects of additional water and hydrogen in CO2 feedstock will be analyzed. Faradic efficiency and chemical selectivity calculated from gas chromatograph and electrochemical analyses will be presented.

Gasb-to-Si Direct Wafer Bonding and Thermal Budget Considerations for Photonic Applications

Extensive progress has been made in recent years in heterogeneous integration (HI) of III-V materials on Si photonics wafers [1], including direct chip-to-chip bonding of GaSb-based infrared (IR) lasers [2], greatly expanding the application space and performance of either material system on its own. This includes active research at Sandia National Labs developing lasers based on GaAs, GaSb, GaN, and InP substrates directly integrated with silicon photonics at the chip and wafer scale. A “device last” process flow is desirable in this case both for scalability and because of the tight alignment tolerance required between the Si waveguides and active III-V laser elements to optimally couple light between the III-V and the Si. In this process flow, the Si photonics wafer is fabricated separately before bonding with an unpatterned III-V wafer or chip. The III-V laser is then defined after bonding, allowing lithographic registration to Si photonics structures. Thus, preparation of both semiconductor surfaces and preservation of the bond between them become critical for device performance and constrain subsequent process steps. Here, we focus on GaSb-based devices.The first consideration is preparing the GaSb and Si surfaces for bonding. Argon sputtering to prepare the GaSb surface for bonding to Si has been investigated, though the emphasis was on GaSb surface roughness, bonding temperature, and electronic transport through the interface [3]. Here, we use x-ray photoelectron spectroscopy (XPS) to investigate the impact of the GaSb oxide composition on the quality of the bond to oxidized Si wafers. In Fig. 1(a)-(c) we use confocal scanning acoustic microscopy (CSAM) to compare as-received 3” GaSb substrates with and without chemical oxide removal to epitaxial GaSb. In the CSAM images, dark areas indicate bond adhesion. We find that bonding improves with decreasing Ga-oxide content realized on the epitaxial GaSb.The second consideration is constraining the laser process steps in order to preserve the bond between the Si photonics and GaSb wafers. Our HI process steps involving GaSb thinning and substrate removal have been described elsewhere [4], though investigation of the thermal budget for survival of the direct GaSb/Si bond through a laser fabrication process flow is lacking in the literature. As the thermal expansion coefficient of GaSb is approximately three times that of Si, temperatures must be limited to prevent the GaSb from expanding excessively and delaminating from the Si wafer when running the III-V laser fabrication after integration with the Si photonics wafer. We investigate the robustness of the bond between epitaxial GaSb and the Si photonics wafer through cross-sectional transmission electron microscopy (TEM) of the bond interface after various process steps typical to laser fabrication and the implications of the thermal budget on these process steps. For example, we find that extended periods of time (more than an hour) at 250°C, which is typical for chemical vapor deposition (CVD) of SiO2 or Si3N4, cause the thinned III-V wafer to delaminate from the Si photonics wafer. While we don’t observe destructive delamination at lower processing temperatures, high-angle annular dark-field imaging (HAADF) analysis in Fig. 1(d) shows significant Sb diffusion into the Si photonics native SiO2 layer.In summary, for optimal performance of GaSb-based hybrid lasers directly bonded to Si photonics, understanding and preserving the bond between these materials is critical. These considerations include minimizing the Ga-oxide at the GaSb surface prior to bonding to promote bond success and keeping extended thermal processes below 250°C to maintain the bond between the GaSb and the Si photonics wafers. These results will inform processes required for full laser fabrication flow, particularly in steps that traditionally require higher or longer temperature parameters.SNL is managed and operated by NTESS under DOE NNSA contract DE-NA0003525.[1] D. Caimi, et al., IEEE Trans. Elect. Dev. 68, p. 3149 (2021).[2] A. Spott, et al., Optica 5, p. 996 (2018).[3] F. Predan, et al., Appl. Surf. Scie., 353, p. 1203 (2015).[4] M. Wood, et al., in CLEO 2023 Technical Digest Series, STh3H.5 (2023). Figure 1

Design and Performance Evaluation of a Specialized Bubbler System for Accurate and Repeatable Solid Oxide Electrolysis Cell (SOEC) Testing

Accurate assessment of Solid Oxide Electrolysis Cell (SOEC) performance demands standardized testing conditions, particularly in stable steam delivery. Fluctuations in steam concentration and flow rate can significantly impact measured open-circuit voltage (OCV) and polarization behavior. Although direct steam injection is straightforward, it is often hindered by instability resulting from intermittent liquid water flux, pressure fluctuations, and fractional distillation effects. Bubbler humidification systems have the potential to offer consistent steam, but tailored designs for SOEC testing are currently absent.This study introduces a specialized bubbler system designed to deliver stable steam to SOEC test stands accommodating both oxygen-conducting (O-SOEC) and proton-conducting (H-SOEC) cells. The bubbler components include a refill water reservoir, a level control module, heating elements, pressure relief valves, check valves, tubing, and fittings integrated with the test stand. The system humidifies the sweep gas, transporting steam to the cell test fixture situated within a high-temperature furnace.The design process involved meticulous considerations of materials compatibility, hydrogen safety, and overtemperature protection. All wetted components employ stainless steel, glass, or PTFE materials in their construction construction. Redundant thermocouples ensure safe process temperatures with automated overtemperature shut off. The refill reservoir and bubbler headspace operate near ambient pressure, facilitated by an exhaust line vent sized for minimal backpressure.In various executed O-SOEC tests, the bubbler maintained OCV stability within ±5 mV over several hundred hours for each cell operating at 750°C, eliminating spikes caused by steam fluctuations observed with direct injection methods. This facilitates precise electrochemical analysis and determination of area-specific resistance losses. Polarization curves align with expected behavior based on the Nernst equation. The system has demonstrated safe and stable functionality for over thousands of hours across various operating conditions.The bubbler design presents researchers with notable advantages over existing steam supply options for SOEC test stands, addressing performance, safety, and flexibility concerns. Online instrumentation enables closed-loop control of steam conditions, enhancing stability. Standardization of test equipment is crucial for quality results, and this work contributes progress toward reproducible protocols in the international SOEC community. The modular bubbler approach, integrated with safety features, also signifies safer methodology choices for lab-scale experimental research.

Water Soluble Poly(amic acid) Binder for Anode Coating and High Temperature Processing

The advent of lithium batteries has been a cornerstone in the evolution of electric vehicle technology, offering a sustainable alternative to fossil fuels and transforming the transportation landscape. The integration of water-soluble binders in the scalable production of anodes significantly enhances the efficiency and sustainability of lithium battery manufacturing. Further advances in battery manufacturing require enhanced tolerance to high temperatures and increased mechanical robustness, especially for high-throughput roll-to-roll production process. In this study, we present a water-soluble poly(amic acid)-based binder, uniquely designed to facilitate aqueous coating processes and withstand high processing temperatures for anode manufacturing. This innovative binder demonstrates remarkable efficiency in securely binding active materials, such as graphite or silicon, ensuring their integrity and performance throughout the battery cycling process.

Water-mediated chelation dynamics of dicarboxylic acid functionalized TiO2 nanoparticles for β-nucleation enhancement in isotactic polypropylene composites

ABSTRACT Isotactic polypropylene (iPP) is the most prominent form of polypropylene, and β-phase is the most resistant to impact compared to the crystalline forms. However, β-phase is the least frequently obtained under conventional operating conditions. TiO2 nanoparticles were functionalized with dicarboxylic acids as nucleating agents to promote β-crystal formation in iPP. The effects of three dicarboxylic acids – glutaric, pimelic, and azelaic – were characterized on TiO2-modified surfaces. Additionally, the interactions between TiO2 and water molecules, crucial for the formation of chelating or bridging linkages, were analyzed using Fourier Transform Infrared spectroscopy. For pimelic and azelaic acids at the polymer processing temperature, the carboxyl group band disappeared, suggesting a transition of the acid-calcium union from a bridging to a chelating linkage due to the presence of water molecules. These molecules help maintain the stability of the chains during processing. X-ray diffraction (XRD) analysis confirmed a higher content of β-crystalline structures in iPP when modified with pimelic and azelaic acids. The research indicates that water molecules, desorbed during manufacturing, facilitate the chelating form, thereby enhancing β-nucleation and improving the surface properties of iPP composites. These β-nucleated PP composites represent a promising material solution for medical device applications, offering a compelling combination of enhanced properties and cost-effectiveness.

High Throughput Manufacturing of Highly Ordered Mesoporous Thin Film Oxides for Hybrid-Polymer Nanocomposite Dielectrics

Highly ordered mesoporous metal oxide thin films have potential to become integrated into widely impactful dielectric materials due to the tunable properties of the oxide and its polymer filling; however, current manufacturing techniques to form the mesoporous oxide greatly limit scalable fabrication. Sol-gel mesoporous metal oxides generated via traditional processes require multi-day aging and high temperature, prolonged curing processes to yield controlled porosity at the expense of manufacturability. Moreover, high cost and unstable alkoxide precursors require precision over the solution precursor pH and subsequent thin film aging humidity after deposition.Solution combustion synthesis (SCS) is a next-generation method of generating metal oxides at reduced process temperatures (often <300 ºC) and using green precursors compared to the sol-gel approach. The metal oxide is typically produced from a metal nitrate, which provides both the metal cation and oxidant and an organic chelator fuel. The fuel acts to stabilize the cation against hydrolysis and to participate in the exothermic redox reaction that results in the metal oxide.Here, we present porogen integrated rapid oxidation (PIRO) which utilizes the principles of SCS to fabricate large-area mesoporous thin films of AlOx in less than 1 hour and at a temperature of 230 ºC. The PIRO method uses low-cost precursors to generate micelles with a controllable open-cell porosity ranging from ~30 – 60% and with varying degrees of closed-packed cubic ordering at a nearly 95% reduction in overall processing time. We show the precursor chemistry can be deposited via ultrasonic spray or blade coating at up to 6 m/min to manufacture large area mesoporous oxides and demonstrate filling of the porous AlOx with TOPAS® polymer to generate a hybrid nanocomposite with a dielectric constant of 6.26.

Pathfinding Process Development for the Realization of Atomic Precision Advanced Manufacturing (APAM)-Based Vertical Tunneling Field Effect Transistors for Enhanced Energy Efficiency

Since the end of Dennard scaling, where metal oxide semiconductor field effect transistor (MOSFET) operating frequency and energy efficiency improved with shrinking device dimensions [1], increasing transistor density is predicted to increase the total power consumption of a system [2]. A key limitation for MOSFETs is that the minimum rate of turn-on, or subthreshold swing (SS), is ~60 mV/decade at room temperature because of the Boltzmann statistics that dictate charge density. Thus, maintaining constant electric field without increasing energy consumption (i.e. gate bias) requires decreasing the SS by investigating alternative materials or device designs, like tunnel FETs (TFETs) [3]. Recent advances in atomic-scale control promise to provide control over quantum mechanical degrees of freedom which have hindered TFET performance in practice. These considerations make atomic precision advanced manufacturing (APAM) an appealing platform to realize a proof-of-concept TFET with atomic scale features [4,5].APAM can produce a 2D sheet of dopants in silicon beyond the solid solubility limit that can be patterned in-plane and capped with epitaxial silicon for strong carrier confinement in the out-of-plane direction (Figure 1). Indeed, improvements to planar TFETs that effectively have 1D channels with low on:off current ratios have been proposed by changing to a vertical geometry that leverages the carrier confinement afforded by 2D materials to create a 2D channel [6], though these materials are not typical in a silicon foundry. In contrast, APAM provides this carrier confinement while exclusively using materials and chemicals that are used in silicon foundries and with compatible processes [7]. In the APAM TFET (Figure 1.8.), a gate bias induces a layer of holes at the oxide/silicon interface that extends from the source, enabling tunneling between the 2D phosphorus-doped layer that comprise the drain and the 2D induced hole layer.As tunnelling occurs vertically through the epitaxial silicon cap, it becomes critical to determine the optimal growth temperature, to keep the dopants in a 2D sheet at low temperatures versus producing low-defect silicon at higher temperatures. Similarly, for optimal electric field control, it becomes critical to determine the optimal processing temperature to maintain the 2D dopant sheet and produce a low-defect gate oxide. The electronic thickness of the dopant layer can be measured using weak localization and the segregation of dopants out of the 2D sheet can be measured using secondary ion mass spectrometry. Our intial attemps at evaluating the electrical quality of the epitaxial silicon cap used PMOS transistors made with an ALD gate dielectric on APAM material without the buried phosphorus layer. Intuitively, we expect material grown at a higher temperature to produce a lower density of defects and therefore more performant PMOS, but find instead that the initial results demonstrate no systematic trend. These results potentially indicate there is an unknown variable obscuring the intentionally changed variable of growth temperature. Here, we propose several possible causes for this observation – both the variability from APAM processing or low-temperature microfabrication could mask an underlying trend.In summary, an APAM TFET provides a path toward increasing energy efficiency of transistors by decreasing SS compared to MOSFETs. The process tradeoffs that produce tightly confined 2D doped layers compared to low defect materials are starting to be explored using PMOS devices. Here, we report on the impact of process variability in drawing conclusions from these devices toward the realization of an APAM TFET.SNL is managed and operated by NTESS under DOE NNSA contract DE-NA0003525.[1] R. H. Dennard et al., “Design of ion-implanted MOSFET's with very small physical dimensions”, IEEE J. Solid-State Circuits 9, 256 (1974).[2] https://irds.ieee.org/[3] J. Koga et al., “Negative differential conductance in three‐terminal silicon tunneling device”, Applied Physics Letters, 69, 1435 (1996).[4] T.-M. Lu et al., “Path towards a vertical TFET enabled by atomic precision advanced manufacturing”, 2021 Silicon Nanoelectronics Workshop (2021).[5] X. Gao et al., “Modeling and Assessment of Atomic Precision Advanced Manufacturing (APAM) Enabled Vertical Tunneling Field Effect Transistor”, 2021 SISPAD, 102 (2021).[6] H. Lu et al., “Tunnel Field-Effect Transistors: State-of-the-Art”, IEEE J. Electron Device Society, 2, 44 (2014).[7] S. Misra et al., “Method of chemical doping that uses CMOS-compatible processes”, U.S. Patent 11,798,808. Figure 1

Preparation of Soft Magnetic Composite Using Cold Sintering Technique

Soft magnetic composites are powder metal products under development as an alternative to 2D laminates in electric motor applications. The 3D design of SMCs offers greater energy efficiency but poses a challenge to maintain adequate strength properties required for application. Soft magnetic composites are fabricated through compaction and heat treatment of iron particles coated with insulated coating to form a dense compact. The soft magnetic properties of the compact are affected by the properties of the iron powder, density of compact as well as the efficacy of forming uniform thin insulating coating at the particle boundary. Additionally, the strength of the compact is also affected by the nature of the insulating boundary at the particle interfaces. We report a low temperature process that involves cold sintering phenomenon to densify and strengthen soft magnetic composites. Iron powders have been modified using a co-precipitation method that forms a hydrated copper/iron oxalate coating on individual iron particles. Warm compaction of the modified iron powders at 100°C resulted in a highly dense soft magnetic composite which demonstrated ~ 3x improvement in strength. The compacts can be further heat treated in air at higher temperatures to form high strength oxide coating iron based soft magnetic composites. Results of the AC and DC magnetic measurements of fabricated cold sintered toroid compacts made as a function of heat treatment temperature reveal that DC permeability increased with heat treatment temperature. Analysis of AC core loss data showed that hysteresis power losses dominated the performance at lower heat treatment temperatures (< 300°C) beyond which dynamic core losses significantly increased.

(Invited) Department of Energy, Energy Efficiency and Renewable Energy - Activity Updates in Reversible Fuel Cells and High Temperature Electrolysis

The Hydrogen and Fuel Cell Technologies Office (HFTO) within the U.S. Department of Energy’s (DOE) Office of Energy Efficiency and Renewable Energy (EERE) supports a range of analysis, research, development, and demonstration efforts that fall under the areas of high temperature electrolysis (HTE) and reversible fuel cells (RFCs). These efforts range from earlier stage R&D on cell components to demonstrating early system technology. Particularly when used in conjunction with high temperature process heat, HTE technology shows promise for highly efficient, cost effective, sustainable hydrogen production at high volumes. This potential has led to its inclusion in multiple HFTO initiatives, including two national lab-led consortia separately focused on next generation materials and overcoming technical barriers to manufacturing durable, affordable, and efficient HTE systems. These consortia objectives, efforts, scopes, and developments are discussed in the context of HTE and recent DOE initiatives and announcements, including the Hydrogen Energy Earthshot, Long Duration Energy Storage Earthshot, and Clean Fuels and Products Earthshot.

Impact of a polysidpersed fuel distribution on the ignition characteristic

Determining the thermal profile of ignition is important because the desired ignition behavior varies with the objective. For example, extended ignition prolongs the time that the engine runs; however, fast ignition offers a higher power gain. The pollution caused by undesirable chemical reactions, as determined by the ignition profile, is another important aspect. Based on a previously developed method, we examined the impact of different theoretical particle size distributions (PSDs) on the thermal ignition profile. We compared different PSDs of polydispersed fuel spray with normal distributions with various means, each corresponding to the same fuel volume. Our results revealed a significant dependence of thermal ignition on the PSD. Systems that comprised only low-radius droplets did not reach ignition, whereas systems with only high-radius droplets required a long time to establish ignition. Moreover, the change in the mean droplet radius unexpectedly resulted in a double hump in the maximum temperature of the combustion process.

Effect of Phosphate-Bridged Monomer on Thermal Oxidative Behavior of Phthalonitrile Thermosets.

Phthalonitrile thermosets are known for their excellent mechanical, physico-chemical, and fire-retardant properties, making them attractive for aerospace and mechanical engineering applications. When producing and applying phthalonitrile-based structural parts, it is essential to consider aspects such as processability and the long-term stability of the material's properties at high temperatures. In our previous studies, we demonstrated that resins containing phosphate-bridged bisphthalonitrile monomers are easily processable due to their low melting temperature and wide processing window. In this study, we investigated the impact of bis(3-(3,4-dicyanophenoxy)phenyl)phenyl phosphate (PPhPN) monomer content on physico-chemical and mechanical properties, thermal stability, and thermal oxidative stability. This research highlights the importance of conducting long-term thermal oxidative aging studies in addition to thermogravimetric analysis to properly assess the stability of thermosets. The findings indicate that adding less than 15% of PPhPN results in the formation of a crystalline phase, which impairs the resin's processability. Conversely, a high PPhPN content reduces the material's thermal oxidative stability. Therefore, based on mechanical and physico-chemical tests after thermal oxidative aging, it can be concluded that a 10-15% concentration of the phosphate-containing monomer enables easy processability of the phthalonitrile resin and provides excellent long-term thermal oxidative stability at temperatures up to 300 °C, while maintaining a flexural strength exceeding 120 MPa and an elasticity modulus of 4.3 GPa.

The effect of tempering time and cooling environment on the corrosion behavior of AA5083‐H111 alloy

AbstractThe tempering process can increase the mechanical properties of the material, such as hardness and impact strength, as well as enhance the corrosion resistance. Therefore, the selection of appropriate tempering time and cooling environment is crucial. This study aims to investigate changes in properties such as hardness, tensile strength, corrosion resistance, and microstructure of AA5083‐H111 alloy after a brief tempering process (30 minutes, 45 minutes and 60 minutes) at 320 °C, followed by cooling in air and water environments. The study found that tempering time and cooling environment significantly affect the mechanical properties and corrosion rate. The results show that samples labeled as S30 and S60 have the highest hardness and impact strength, but the best corrosion resistance is achieved in the S60 sample. This study demonstrates that even after a limited‐term tempering process, the mechanical properties and corrosion resistance of AA5083‐H111 alloy can be improved. This information is crucial data for use in the production and application of alloys. The findings of this study could have important implications for the production and application of AA5083‐H111 alloy in industries such as aerospace, automotive, and marine engineering.

Impact of Thermochemical Treatments on Electrical Conductivity of Donor-Doped Strontium Titanate Sr(Ln)TiO3 Ceramics.

The remarkable stability, suitable thermomechanical characteristics, and acceptable electrical properties of donor-doped strontium titanates make them attractive materials for fuel electrodes, interconnects, and supports of solid oxide fuel and electrolysis cells (SOFC/SOEC). The present study addresses the impact of processing and thermochemical treatment conditions on the electrical conductivity of SrTiO3-derived ceramics with moderate acceptor-type substitution in a strontium sublattice. A-site-deficient Sr0.85La0.10TiO3-δ and cation-stoichiometric Sr0.85Pr0.15TiO3+δ ceramics with varying microstructures and levels of reduction have been prepared and characterized by XRD, SEM, TGA, and electrical conductivity measurements under reducing conditions. The analysis of the collected data suggested that the reduction process of dense donor-doped SrTiO3 ceramics is limited by sluggish oxygen diffusion in the crystal lattice even at temperatures as high as 1300 °C. A higher degree of reduction and higher electrical conductivity can be obtained for porous structures under similar thermochemical treatment conditions. Metallic-like conductivity in dense reduced Sr0.85La0.10TiO3-δ corresponds to the state quenched from the processing temperature and is proportional to the concentration of Ti3+ in the lattice. Due to poor oxygen diffusivity in the bulk, dense Sr0.85La0.10TiO3-δ ceramics remain redox inactive and maintain a high level of conductivity under reducing conditions at temperatures below 1000 °C. While the behavior and properties of dense reduced Sr0.85Pr0.15TiO3+δ ceramics with a large grain size (10-40 µm) were found to be similar, decreasing grain size down to 1-3 µm results in an increasing role of resistive grain boundaries which, regardless of the degree of reduction, determine the semiconducting behavior and lower total electrical conductivity of fine-grained Sr0.85Pr0.15TiO3+δ ceramics. Oxidized porous Sr0.85Pr0.15TiO3+δ ceramics exhibit faster kinetics of reduction compared to the Sr0.85La0.10TiO3-δ counterpart at temperatures below 1000 °C, whereas equilibration kinetics of porous Sr0.85La0.10TiO3-δ structures can be facilitated by reductive pre-treatments at elevated temperatures.

Process–Property Correlation in Sustainable Printing Extrusion of Bio-Based Filaments

This study investigated the effect of two critical variables for environmental process sustainability, i.e., extruder temperature and printing rate, on thermomechanical performance and accuracy in overall sample sizes, when printing bio-based materials. In this context, 3D specimens produced from basic polylactide (n-PLA) and wood-filled PLA polymer (f-PLA) were realized using extrusion-based additive manufacturing technology (MEX) by varying the nozzle temperatures (200 °C, 210 °C, and 220 °C) and speed (from 70 mm/s to 130 mm/s). Dynamic mechanical analysis (DMA) was carried out on the produced specimens, providing information on changes in storage modulus at testing temperature of 30 °C (E′30) and glass transition temperature (Tg) for each printing condition. Measurements of sample sizes allowed for printing precision considerations as a function of processing temperature and speed. The results revealed similar trends in E′30 changes in printed specimens at a fixed extruder temperature as a function of printing speed for n-PLA and f-PLA. Infrared spectroscopy was performed on printed samples and unextruded material to attest potential material degradation under various operating conditions. Finally, images of sample surface allowed to verify the homogeneity of the diameter of the extruded material, and the layer–layer contact at the interface.

Phosphorus Fraction in Hydrochar from Co-Hydrothermal Carbonization of Swine Manure and Rice Straw: An Optimization Analysis Based on Response Surface Methodology

Livestock manure and crop residues are significant sources of phosphorus. However, the ineffectiveness of current processing technologies often leads to the suboptimal recovery of this phosphorus, causing considerable resource wastage and environmental pollution. Recently, global research has increasingly been focused on the resource recovery of organic waste materials using hydrothermal carbonization technology. This study investigated variations in phosphorus forms in the hydrochar produced from swine manure and rice straw, employing diverse hydrothermal carbonization conditions and applying the Box–Behnken response surface methodology and Hedley’s phosphorus fractionation method. The results indicated that inorganic phosphorus predominates in the hydrochar, with organic phosphorus comprising 5–30% of the total phosphorus. Furthermore, the study found that the available phosphorus content, as measured by NaHCO3 extraction, decreased as the reaction time and temperature of the hydrothermal carbonization process increased. The concentrations of H2O-P and NaHCO3-P fractions decreased with increasing reaction times and temperatures but increased with a higher swine manure-to-straw ratio. Conversely, the concentrations of NaOH-P and HCl-P fractions showed an increasing trend with rising reaction temperature, prolonging reaction time, andusing a high swine manure-to-straw ratio. Consequently, this study offers vital theoretical and practical insights into the resource utilization of livestock manure and crop straw, significantly contributing to the challenges of waste management and environmental sustainability in agriculture.

Effect of Austempering Go-Kart Rear Axle on Toughness Properties and Microstructure Morphology

A Go-Kart is a four-wheeled vehicle that exhibits characteristics similar to a motorcycle. Additionally, since Go-Kartslack shock absorbers, it is crucial to use an engine that minimizes vibrations. The shaft, a typically circular rotating part, is oftenattached to elements like gears and endures continuous loads, which can lead to breakage. Shaft failures are common and often result from incidents caused by the need to use lightweight materials for faster performance. This study aims to examine the strength characteristics of the Go- Kart rear wheel shaft made from ASTM A414 Grade A steel after undergoing bending tests, impact tests, and microstructure analysis. Specifically, it investigates the effects of temperature on the toughness and curvature of the Go-Kart rear wheel shaft post-normalizing and tempering processes. Methods employed include heat treatment, three-point bending tests, Charpy impact tests, and ASTM E3-11 microstructure analysis. The highest impact value, 0.644joules/mm2, was observed in specimen B, which underwent a normalizing process at 850°C and tempering at 300°C. The lowest impact value, 0.190 joules/mm2, was found in specimen A, which underwent a normalizing process at 800°C and tempering at 250°C. The highest three-point bending strength, 2520.1 N/mm2, was also recorded in specimen B, while the lowest, 2255.4 N/mm2, was in specimen C, which underwent normalizing at 900°C and tempering at 350°C. Microstructure analysis revealed that higher temperatures during the normalizing and tempering processes result in the formation of more pearlite crystals and a denser microstructure.

Synthesis of antibacterial fluorescent carbon dots and green coal-like hydrochar from tea Industry byproducts via hydrothermal carbonization

This study introduces an experimental framework employing hydrothermal carbonization (HTC) for the valorisation of factory tea waste as a solid fuel. Employing a centre composite design and response surface methodology, the investigation systematically assesses the influence of two critical process parameters, temperature (180–220 °C) and time (0–240 min), on higher heating value (HHV), hydrochar yield, and energy yield. The study identifies an optimized HTC condition (220°C, 55 min) resulting in the recorded HHV of 22.26±1.10 Mj/Kg. Combustion characteristics and kinetics of the factory tea waste-derived hydrochar (TW-hydrochar) is analysed through TGA and DTG, complemented by structural elucidation via FTIR and FE-SEM. Concurrently, the study reports the observation of carbon dots (TW-CDs) generation during TW-hydrochar production, characterized comprehensively through UV–visible spectroscopy, TEM, XRD, XPS, Zeta potential, and fluorescence methods. Further, antimicrobial properties of TW-CDs are rigorously investigated against Bacillus subtilis and Escherichia coli, manifesting pronounced antibacterial activity against B. subtilis and E. coli as evidenced by a 12 mm and 11 mm inhibition zone, respectively. This research contributes to the scientific understanding of tea waste valorization through HTC, providing insights into cleaner fuel options and the emergence of carbon dots with potential antibacterial applications.