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Development of transparent, particle‐loaded photoresins for volumetric additive manufacturing of silica glass

Abstract Additive manufacturing of glass aims to change the paradigm of glass manufacturing by allowing for improved customization coupled with lower energy and post‐processing needs. Fabrication of glass via volumetric additive manufacturing (VAM) involves printing in a silica‐loaded photopolymer resin with subsequent thermal processing and adds additional advantages by allowing for rapid printing of parts with smooth surfaces and no supports. Previous work in glass VAM has demonstrated fabrication of optical quality microoptics with overall dimensions on the scale of tens of cubic millimeters. For applications requiring glass printed on the scale of cubic centimeters the rheology, scattering, and green part strength must be controlled via resin formulation. Here, we present insight into a novel glass photopolymer resin suitable for VAM and in the effect of tuning formulation on the ability to produce dense glass parts with volumes on the scale of cubic centimeters.

Myers, Luke A.↗

Additive Manufacturing – A New Challenge for Automation and Robotics

Additive manufacturing (AM) is a rapidly growing technology descended from the first stereolithography systems. AM describes a variety of material deposition technologies for forming objects in a digital manner layer-by-layer under computer control. Now commonly known as 3D printing, AM quickly branched out into several key directions – material extrusion, sheet lamination, direct energy deposition, vat polymerization, powder bed fusion, binder jetting, and material jetting. The common factor in all AM branches is a foundation in robotics and automation. While most of the mechanical 3D printing structures are based on simple gantry systems, there are Gough-Stewart platforms and, more recently, six or more DoF manipulator-based systems that have been developed. Currently available commercial systems are based on open-loop control with minimum sensing capabilities; the latest systems in development are starting to take advantage of complex feedback loops and layers of advanced sensing and data logging. The Manufacturing Demonstration Facility of Oak Ridge National Laboratory is leading the efforts in applying advanced robotics in the creation of large-scale 3D printers. The recent demonstration of an additively manufactured excavator at the CONEXPO 2017 exhibition in Las Vegas showed that the use of cutting edge robotics and automation is essential for the next generation of additive systems. The future of AM will heavily rely on advanced robotics, machine learning, and the internet of things. This paper summarizes progress in AM; presents the practical aspects, challenges, and lessons learned in developing robotic-based AM systems; and outlines the needs and future directions of robotics for AM.

Nycz, Andrzej↗

On the potential mechanisms of β to α' + β decomposition in two phase titanium alloys during additive manufacturing: a combined transmission Kikuchi diffraction and 3D atom probe study

In this paper, we focus on the mechanisms of phase transformations in additively manufactured Ti–6Al–4V during cooling. In particular, the goal is to understand if the imposed thermal cycles during fabrication results in the complete transformation of the α' to the β phase or the sub-transus decomposition of α' (martensite) to α + β. To this effect, samples fabricated using electron beam melting and laser-directed energy deposition techniques were analyzed using atom probe tomography (APT) in conjunction with correlative transmission Kikuchi diffraction (TKD). While the composition measurement using APT shows partitioning of vanadium into the β phase, the crystallographic analysis suggests evidence of a shear-induced transformation. Despite the pronounced differences in the processing conditions, both of the additive manufacturing techniques lead to similar partitioning of vanadium to the β phase. Finally, calculations using THERMOCALC and DICTRA show that under the time and temperature regimes of additive manufacturing the microstructure could develop by the decomposition reaction of α' → α+β.

36 MATERIALS SCIENCE↗

Reinforcement of Soy Protein-Based Bioplastics Through Addition of Lignocellulose and Injection Molding Processing Conditions

Bioplastics have gained great interest in recent years as a potential alternative to conventional plastics, since they are renewable and biodegradable materials. However, their mechanical properties are not able to match those of conventional plastics yet. In this context, the incorporation of additives to improve those properties of bioplastics is an interesting line of research. The aim of this work was to develop soy protein-based bioplastics with lignocellulosic fiber (additive) by injection molding. Mechanical and absorption properties of bioplastics reinforced with lignocellulose (0.1, 1.0, 5.0 wt%) have been studied, as well as their microstructure. Furthermore, a study of the effect produced by changing the mold temperature (70, 90, 110, 130 °C) was carried out. The results obtained confirm an improvement of the mechanical properties of these bioplastics, depending on the amount of fiber incorporated. In any case, these findings support the role of cellulosic compounds as additives in protein bioplastics.

36 MATERIALS SCIENCE↗

The Additive Approximation for Heat Transfer and for Stability Calculations in a Multi-filamentary Superconductor - part A

This paper addresses the applicability of the “additive approximation” of total thermal conductivity in heat transfer and in superconductor stability calculations. If cases (a), (b) and (c) denote total (conductive plus radiative), or only conductive or only radiative heat flux, respectively, each flux q-dot calculated with Fourier’s conduction law using the corresponding thermal conductivity (λ{sub a}, λ{sub b}, λ{sub c}), the additive approximation would be confirmed if the heat flux difference Δ q-dot = q-dot {sub a}− q-dot {sub b}− q-dot {sub c}, at any position of an investigated object, and at any time, converges to zero. This is not trivial because of the strong, non-linear temperature dependence of the radiation component. Heat transfer calculations including radiative transfer are presented in this paper, first for simple, homogeneous, thin film test samples and later for a multi-filamentary BSCCO 2223 superconductor. The simulated heat sources either result from a sudden increase of conductor boundary temperature or from flux flow and Ohmic resistances in the superconductor under a disturbance (like transport current exceeding critcal current density). The conductors, though very thin, are non-transparent to mid-IR radiation. Validity of the additive approximation is critical for superconductor stability against quench. Based on the applied numerical scheme, a hypothesis is suggested concerning correlation of the results of the simulation (the “numerical space”) with the experimental situation (the “physical reality”): Non-convergence of the numerical scheme might tightly be correlated with occurrence of a quench in the simulated superconductor.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Temperature-Dependent Thermal and Mechanical Properties of a Wire Arc Additively Manufactured Low Transformation Temperature Steel

Recent research has studied the use of low transformation temperature (LTT) martensite steel as feedstock for wire arc additive manufacturing (WAAM) and low tensile residual stresses or compressive residual stresses were detected in the printed walls. These residual stress states help to improve printed product properties such as fatigue strength and corrosion resistance. However, the thermal and mechanical properties of WAAM printed LTT martensite steel walls are largely unknown. In this work, a printed LTT martensite steel was characterized for its thermal, metallurgical, and mechanical behavior at room and elevated temperatures. The temperature-dependent specific heat capacity, thermal expansion, atomic lattice spacing, and tensile properties were measured during both heating and cooling and related to observed microstructural features and computational thermodynamics predictions. These results revealed a large hysteresis in the martensitic transformation, with a martensite start temperature of 240 °C and austenite start temperature of 680 °C. Additional thermal cycles and specimen orientation did not affect the printed specimen austenite and martensite transformations. However, it was observed that the printed metal may exhibit tempering embrittlement at about 350 °C but further studies are needed to confirm that. Further, these results suggest that a temperature control of 250 °C to 350 °C during WAAM is needed to maximize the stress reduction potential of the LTT250 martensite steel. Opportunities for future implementation of LTT martensite steels and optimization of additive manufacturing process conditions are identified.

36 MATERIALS SCIENCE↗

Advanced Process Possibilities in Friction Crush Welding of Aluminum, Steel, and Copper by Using an Additional Wire

Joining sheet metal can be problematic using traditional friction welding techniques. Friction crush welding (FCW) offers a high speed process which requires a simple edge preparation and can be applied to out-of-plane geometries. In this work, an implementation of FCW was employed using an additional wire to weld sheets of EN AW5754 H22, DC01, and Cu-DHP. The joint is formed by bringing together two sheet metal parts, introducing a wire into the weld zone and employing a rotating disk which is subject to an external force. The requirements of the welding preparation and the fundamental process variables are shown. Thermal measurements were taken which give evidence about the maximum temperature in the welding center and the temperature in the periphery of the sheet metals being joined. The high welding speed along with a relatively low heat input results in a minimal distortion of the sheet metal and marginal metallurgical changes in the parent material. In the steel specimens, this FCW implementation produces a fine grain microstructure, enhancing mechanical properties in the region of the weld. Aluminum and copper produced mean bond strengths of 77 and 69 pct to that of the parent material, respectively, whilst the steel demonstrated a strength of 98 pct. Using a wire offers the opportunity to use a higher-alloyed additional material and to precisely adjust the additional material volume appropriate for a given material alignment and thickness.

36 MATERIALS SCIENCE↗

Left ventricular ejection fraction determined with the simulation of a very low-dose CZT-SPECT protocol and an additional count-calibration on planar radionuclide angiographic data

Purpose: To determine whether the left ventricular ejection fractions (EFs), measured on a high-sensitivity CZT single photon emission computed tomography (SPECT)-camera with a 70% reduction in recording times and a prevention of EF overestimation through an additional count-calibration, are concordant with reference EF from planar radionuclide angiography (2D-RNA). Methods: An additional 10-minute CZT-SPECT recording was performed in patients referred to 2D-RNA for cardiomyopathy (n = 23) or chemotherapy monitoring (n = 50) with an in vivo red blood cell labeling with 850 MBq {sup 99m}TcO{sub 4}{sup −}. The EF, obtained from CZT-SPECT with 100% (SPECT100) or 30% (SPECT30) projection times and with a SPECT-count calibration on the 2D-RNA counts of corresponding cavity volumes, were compared to EF from 2D-RNA. Results: Strong and equivalent relationships were documented between the EF from 2D-RNA and the calibrated EF from SPECT100 (y = 0.89x + 6.62; R{sup 2} = 0.87) and SPECT30 (y = 0.87x + 8.40; R{sup 2} = 0.85), and the mean EF from SPECT100 (54% ± 15%) and SPECT30 (53% ± 16%) were close to that from 2D-RNA (55% ± 15%). However, upward shifts in these mean values were documented in the absence of count calibration for both SPECT100 (60% ± 18%) and SPECT30 (60% ± 18%). Conclusion: Left ventricular EF may be determined on a high-sensitivity CZT-camera, a 70% reduction in injected activities, and an additional count-calibration for further enhancing the concordance with 2D-RNA values. [French] French Abstract: Objectif: Déterminer si les fractions d'éjection ventriculaire gauche (EF) mesurées sur une caméra CZT SPECT à haute sensibilité avec une réduction de 70% des temps d'enregistrement et une prévention de la surestimation de l'EF grâce à un étalonnage supplémentaire des coups concordent avec les EF de référence obtenues par angiographie scintigraphique planaire (2D-RNA). Méthodes: Un enregistrement CZT-SPECT supplémentaire de 10 minutes a été réalisé chez les patients référés pour évaluation de cardiomyopathie (n=23) ou suivi de chimiothérapie (n = 50) par angiographie scintigraphique planaire (2D-RNA) au globules rouges marqués avec 850 MBq 99mTcO4-. Les EF, obtenues au moyen d’une caméra CZT-SPECT avec 100% (SPECT100) ou 30% (SPECT30) de temps d’acquisition et avec étalonnage des coups SPECT sur les images 2D-RNA des volumes de cavité correspondants ont été comparés aux EF à partir de 2D-RNA. Résultats: une corrélation significative existe entre les EF obtenues par 2D-RNA et les EF étalonnées obtenues par SPECT100 (y = 0,89x + 6,62; R2 = 0,87) et SPECT30 (y = 0,87x + 8,40; R2 = 0,85). Les EF moyennes de SPECT100 (54 ± 15%) et SPECT30 (53 ± 16%) sont similaires à celles obtenues par 2D-RNA (55 ± 15%). En l'absence d'étalonnage de comptage des études SPECT100 (60 ± 18%) et SPECT30 (60 ± 18%), ces valeurs moyennes d’EF sont généralement plus élevées. Conclusion: La fonction ventriculaire gauche peut être déterminée avec une caméra CZT à haute sensibilité, une réduction des activités injectées et un étalonnage supplémentaire des coups pour améliorer la concordance avec les valeurs obtenues par 2D-RNA. [Spanish] Spanish Abstract: Propósito: Determinar si la fracción de eyección del ventrículo izquierdo, medida con la cámara CZT-SPECT con una reducción del 70% en tiempo de grabación y con la prevención de la sobreestimación mediante una calibración de cuentas adicional, que sea concordante con el valor referencia de fracción de eyección mediante radiografía planar de radionucleidos. (2D-RNA). Métodos: Una grabación adicional de 10 minutos con CZT-SPECT se realizo en pacientes referidos a radiografía planar de radionucleidos (2D-RNA) por miocardiopatías. (n = 23) o para monitorizar las quimioterapias (n = 50) con marcaje de glóbulos rojos con 850 MBq 99m TcO4. La fracción de eyección obtenida por CZT-SPECT con 100% (SPECT100) o 30% (SPECT30) de tiempo de proyección, y con SPECT con calibración de cuentas con el 2D-RNA, los volúmenes de cavidades fueron comparados con fracción de eyección . Relaciones fuertes y equivalentes fueron documentados entre fracción de eyección del 2D-RNA, y la forma calibrada de la fracción de eyección SPECT100 (y = 0.89x + 6.62; R2 = 0.87) y SPECT30 y = 0.87x + 8.40; R2 = 0.85), y la media de fracción de eyección de SPECT100 (54 ± 15%) and SPECT30 (53 ± 16%) fueron cercanos a la de el 2D-RNA (55 ± 15%). Aunque, aumentos en estas medias se documentaron en la ausencia de la calibración de cuentas para SPECT100 (60 ± 18%) y SPECT30 (60 ± 18%). Conclusión: La fracción de eyección del ventrículo izquierdo puede ser determinada con una cámara CZT de alta sensibilidad, una reducción del 70% en actividades inyectadas y la calibración de cuentas adicional para realzar la concordancia con los valores de 2D-RNA. [Chinese] Chinese Abstract: 目的: 以平面放射性核素血管造影 (2D-RNA) 测定左心室射血分数 (EF) 作为参考标准,为确定利用高灵敏度 CZT SPECT 相机在减少 70% 的记录时间, 并结合计数校准防止高估情况下测量的 EF值, 是否与 2D-RNA 测得的 EF 值一致。 方法: 对心肌病 (n = 23) 或化疗监测 (n = 50) 的患者采用体内标记法注射 850 MBq {sup 99m}TcO{sub 4} 标记的红细胞进行 2D-RNA ,随后再采集 10 分钟 CZT-SPECT。 对 CZT-SPECT 100% 投影时间 (SPECT100) 或 30% 投影时间 (SPECT30) 获得的图像进行重建, 并进行计数校准 (对相应容积获得的 2D-RNA 计数通过 SPECT 校准)获得 EF 值, 与 2D-RNA 测定的 EF 的进行比较。 结果: 2D-RNA 测定的 EF 值与 SPECT100 校准后测定的 EF 值 (y = 0.89x + 6.62; R{sup 2} = 0.87) 及 SPECT30 (y = 0.87x + 8.40; R{sup 2} = 0.85) 校准后 EF 值具有高度相关性, 并且 SPECT100 (54 ± 15%) 和 SPECT30 (53 ± 16%) 测定的 EF 平均值与 2D-RNA 测定的 EF 平均值 (55 ± 15%) 非常接近。 但是, 在没有计数校准的情况下, SPECT100 (60 ± 18%) 和 SPECT30 (60 ± 18%) 测定的 EF 平均值会被高估。 结论: 高灵敏度 CZT 相机可在减少 70% 的注射剂量情况下测定左心室 EF 值, 结合计数校准可进一步提高与 2D-RNA测得的 EF 值的一致性。 关键词: 放射性核素血管造影; 血池 SPECT; CZT 相机; 左心室射血分数; 校准曲线。.

62 RADIOLOGY AND NUCLEAR MEDICINE↗

Validation Data for Benchmarking Wire Arc Additive Manufacturing Process Simulations

Residual stresses cause geometric distortion and affect mechanical performance of additively manufactured structures, yet they are notoriously difficult to assess and predict. Distortion (warpage) can drive parts outside dimensional tolerance limits, leading to part rejection or rework. For parts that meet tolerance, locked-in residual stress fields can affect structural integrity during operation, particularly subcritical cracking by fatigue, creep, or corrosion. This work develops benchmark data for a common additive manufacturing process (Wire Arc Additive Manufacturing) that can be applied for calibration and validation of physical process models that predict residual stress fields. The work includes design of two different samples of differing geometry, detailed manufacturing records for a set of physical samples, and an extensive set of residual stress measurement data developed using two diverse techniques (the contour method and neutron diffraction). An initial application of the work is also reported, where a modeling challenge was issued to secure residual stress model predictions from two independent laboratories that were blind to residual stress measurement data. These initial blind residual stress predictions show significant discrepancies relative to the measurement data, illustrating the potential value of the underlying validation data. An open repository for this work, including the sample designs, manufacturing process records, and the residual stress data, is also provided for future application in non-blind validation efforts.

36 MATERIALS SCIENCE↗

Additive Manufacturing in the Nuclear Reactor Industry

This article discusses the application of additive manufacturing in the nuclear reactor industry.Additive manufacturing for nuclear applications increased significantly in the late 2010s due to rapid progress in technology, particularly with methods using metals and ceramics.Because these manufacturing technologies are uniquely data-rich, they allow for an advanced understanding of materials, and they offer the potential to predict part performance based on build data. The inherent characteristics of additive manufacturing technologies allow for rapid prototyping and geometric freedom, making it possible to implement an accelerated agile design process for advanced nuclear reactor applications. Predictive high-fidelity multiphysics simulations are crucial to fully leverage this geometric flexibility. Qualification and regulator acceptance ultimately determine the breadth and scope of applications for these technologies. The US Department of Energy Office of Nuclear Energy Transformational Challenge Reactor program integrates many of these elements to accelerate the deployment of additive manufacturing technologies to industry.

Betzler, Benjamin↗

Microstructural evolution during quenching and partitioning of 0.2C-1.5Mn-1.3Si steels with Cr or Ni additions

Here, the influence of Cr and Ni additions and quench and partition (Q&P) processing parameters on the microstructural development, including carbide formation and austenite retention during Q&P, was studied in two steels with a base composition of 0.2C-1.5Mn-1.3Si wt.% and additions of 1.5 wt.% Cr (1.5Cr) or Ni (1.5Ni). Additions of 1.5 wt.% Cr significantly slowed the kinetics of austenite decomposition relative to the 1.5Ni alloy at all partitioning temperatures, promoting greater austenite retention, lower retained austenite carbon (C) contents, and reduced sensitivity of the retained austenite amounts to processing variables. In the 1.5Cr alloy after partitioning at 400 °C for 300 s, η-carbides were identified by transmission electron microscopy (TEM) and atom probe tomography (APT) revealed no significant enrichment of substitutional elements in the carbides. In the 1.5Ni alloy after partitioning at 450 °C for 300 s, both plate-like and globular carbides were observed by TEM. APT analysis of the globular carbides clearly revealed significant Si rejection and Mn enrichment. Mössbauer effect spectroscopy was used to quantify the amount of carbides after Q&P. In general, carbide amounts below ~0.3% of Fe were measured in both alloys after partitioning for short times (10 s), irrespective of quench or partitioning temperature, which corresponds to a relatively small portion of the bulk C. With increasing partitioning time, carbide amounts remained approximately constant or increased, depending on the alloy, quench temperature, and/or partitioning temperature.

36 MATERIALS SCIENCE↗

Large Format Composite Additive Manufacturing for Low-Head Hydropower

Hydropower with a small elevation change from inlet to outlet, known as “low-head” hydropower, is a relatively untapped resource for reliable green power generation. One major barrier to entry is the cost of the components needed to generate the power. Each installation site is unique, with various head levels, flow rates, and other unique site characteristics that drive up the cost of development and installation. As a result, custom-made components are necessary because the sites are intrinsically inefficient. However, customized parts are generally more expensive to manufacture than ready-made parts. Often times, the cost of custom-made components is so high that the low-head hydropower installation becomes non-viable. Additive manufacturing offers the ability to make custom components, ideal for one-off applications, at low costs that are well suited for the needs of low-head hydropower. Indirect additive manufacturing, such as making tools or dies rather than end use components, can also be used to make low-cost composite tooling as needed for these custom applications. This paper explores the use of additive manufacturing, both directly and indirectly, to produce the components of a turbine system for a low-head hydropower site. The parts were designed to form a unique modular system, which saves time for future designs and iterations. The system has operated for more than three years without failure at a test site in Wisconsin, USA. This work serves as a basis for future application of AM to low-head systems, in which the modular components can be customized for each unique hydropower installation.

36 MATERIALS SCIENCE↗

Designing for Big Area Additive Manufacturing

Additive manufacturing (AM), more commonly referred to as 3D printing, is revolutionizing the manufacturing industry. With any new technology comes new rules and guidelines for the optimal use of said technology. Big Area Additive Manufacturing (BAAM), developed by Cincinnati Incorporated and Oak Ridge National Laboratory’s Manufacturing Demonstration Facility, requires a host of new design parameters compared to small-scale 3D printing to create large-scale parts. However, BAAM also creates new possibilities in material testing and various applications in the manufacturing industry. Most of the design constraints of small-scale polymer 3D printers still apply to BAAM. Beyond those constraints, new rules and limitations exist because BAAM’s large-scale system significantly changes the thermal properties associated with small-scale AM. Here, this work details both physical and software-related design considerations for additive manufacturing. After reading this guide, one will have a better understanding of slicing software’s capabilities and limitations, different physical characteristics of design and how to apply them appropriately for AM, and how to take the inherent nature of AM into consideration during the design process.

36 MATERIALS SCIENCE↗

Additive manufacturing of two-phase lightweight, stiff and high damping carbon fiber reinforced polymer microlattices

Carbon fiber reinforced polymer (CFRP) composite is known for its high stiffness-to-weight ratio and hence is of great interest in several engineering fields such as aerospace, automotive, defense, etc. However, such a composite is not suitable for energy dissipation as failure occurs with very little or no plastic deformation. Herein, we present an extendable multi-material projection microstereolithography process capable of producing carbon-fiber-reinforced cellular materials that achieve simultaneously high specific stiffness and damping coefficient. Inspired by the upper bounds of stiffness-loss coefficient in a two-phase composite, we designed and additively manufactured CFRP microlattices with soft phases architected into selected stiff-phase struts. Our results, confirmed by experimental and analytical calculations, revealed that the damping performance can be significantly enhanced by the addition of only a small fraction of the soft phase. The presented design and additive manufacturing strategy allow for optimizing mutually exclusive properties. As a result, these CFRP microlattices achieved high specific stiffness comparable to commercial CFRP, technical ceramics, and composites, while being dissipative like elastomers.

36 MATERIALS SCIENCE↗

Impact of controlled prewetting on part formation in binder jet additive manufacturing

Binder jetting is an additive manufacturing process that bonds powder through selectively depositing binder by inkjet printing. The part is then extracted and densified by sintering and/or infiltration. The process offers low costs and fast build rates, but properties can be poor due to residual porosity after sintering. The inkjet printing process may contribute to this residual porosity by creating large pores. The droplet kinetic energy ejects some powder particles from the bed and rearranges others. Particle ejection and rearrangement are theorized to create porous regions in binder-jetted parts. In this work, small amounts of moisture are added to the spread powder before printing and the impact on part formation, part properties, and printing parameters measured with varied droplet spacing, droplet velocity, and print frequency. Moisture is added by applying an atomized fluid mixture to the powder between layer spreading and binder printing. The fluid mixture partially evaporates but leaves a stable residue to increase cohesion and enhance imbibition. Moisture addition to the powder increases the range of droplet spacings for line formation while reducing particle ejection, powder rearrangement, and balling in layer and multilayer parts. Excessive moisture addition decreases the effective saturation of printed lines, but saturation in 3D parts is less impacted. Increased surface roughness in the first few layers of a print was also mitigated with prewetting. Finally, high-speed X-ray imaging verified prewetting reduction in particle ejection and rearrangement.

36 MATERIALS SCIENCE↗

Operando visualization of porous metal additive manufacturing with foaming agents through high-speed x-ray imaging

Porous metals find extensive applications in soundproofing, filtration, catalysis, and energy-absorbing structures, thanks to their unique internal pore structure and high specific strength. In recent years, there has been an increasing interest in fabricating porous metals using additive manufacturing (AM), leveraging its unique advantages, including improved design freedom, spatial material control, and cost-effective small-batch production. In this study, we conducted pioneering operando visualization of AM porous metal using a laser powder bed fusion (L-PBF) setup combined with a high-speed synchrotron x-ray imaging system. Single track printing experiments using Ti6Al4V (Ti64) combined with titanium hydride (TiH 2 ) and sodium carbonate (Na 2 CO 3 ) as foaming agents, with varying mixing ratios were performed under different processing conditions. Here. the results elucidate the dynamic development of porosity formation. The average pore size is significantly influenced by the particle size of foaming agents when pore coalescence is absent. For all foaming agent content tested in the current study, the number of pores is found to be more sensitive to changes in laser power than in laser scanning speed. Increasing linear energy density (increasing laser power or reducing laser scanning speed) promotes the foaming agent activation thereby porosity formation. However, high linear energy density skews pore distribution towards the surface despite forming deeper melt pools. In addition, the impact of additional factors including foaming agent's laser absorptivity and decomposition kinetics with respect to AM time scales should be carefully considered to avoid ineffective activation of foaming agents during the AM of porous metals.

36 MATERIALS SCIENCE↗

Tailoring biogenic straw insulation from additive manufacturing

In the pursuit of carbon-storing materials that could help accomplish high levels of building sustainability, wheat straw has emerged as a promising alternative to fossil fuel-based building materials. Straw is 100% biodegradable and abundant agricultural waste used in the construction 400 years ago, and it has been reported to have the lowest embodied carbon when measured against other typical insulating materials. Here, in this study, we report additive manufacturing of carbon-sequestration insulation panel materials by upcycling cellulose fibrils from wheat straw. Cellulose obtained from alkaline and 2,2,6,6-tetramethylpiperidine-1-oxyl radical-mediated oxidation shows thermal conductivity of 0.036 W m -1 K -1 , alongside elastic and flexural modulus of 900 MPa and 502 MPa, respectively. In addition, an in-situ hydrophobic treatment in the cellulose-based insulation panels is achieved with an average water contact angle of 133.7° Furthermore, the extrusion-based additive manufacturing of a 3D-printable ink obtained by mixing the cellulose and silica aerogel precursor is accomplished, with the printed material exhibiting structural integrity, thus showing great potential towards the development of state-of-the-art, sustainable materials for carbon-sequestration building applications.

36 MATERIALS SCIENCE↗

Coupled methane and NO x conversion on Pt + Pd/Al 2 O 3 monolith: Conversion enhancement through feed modulation and Mn 0.5 Fe 2.5 O 4 spinel addition

The performance of a dual-layer Pt-Pd/Al 2 O 3 washcoated monolith promoted by an Al 2 O 3 -supported Mn 0.5 Fe 2.5 O 4 spinel base layer was evaluated with the objective to develop a catalyst with a lower loading of Platinum group metal (PGM) for stoichiometric natural gas vehicle (NGV) emission control. Flow reactor results show that a combination of a lean/rich modulated feed and spinel addition gives enhanced methane and NO conversions compared to a steady-state feed having the same overall composition. Washcoated catalysts – PGM-only, spinel-only, PGM + spinel – were compared over a wide range of operating conditions. The results show a decrease in the methane conversion light-off temperature of up to 85 °C for an application-relevant feed (CH 4 + NO + H 2 + CO + O 2 + H 2 O + CO 2 ) while a moderate 40 °C decrease was observed for a simple feed (CH 4 + O 2 + H 2 O + CO 2 ). In the absence of spinel the modulation enhancement is negatively impacted at high methane conversion (> 80 %). The data show that the O 2 storage and release property of the spinel is needed to fully exploit the modulation enhancement. The mechanism responsible for the enhancement is linked to suppression of O 2 inhibition on the methane oxidation rate near the stoichiometric neutral point (λ = 1). Sufficiently fast cycling achieves a balance between a metallic and oxidic precious metal crystallites favorable for methane activation. The addition of spinel moves this balance closer to the λ = 1 feed, enabling a high oxidation efficiency with lower byproduct NH 3 selectivity. Enhancement in the NO conversion follows the methane conversion due to an easier NO reduction under the slightly rich of stoichiometric feed. Comparison of the PGM + spinel catalysts to PGM-only catalysts shows that the addition of spinel in combination with modulation can achieve the same activity with a lower PGM loading.

03 NATURAL GAS↗