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At least 505 records · Page 28

Investigating Sintering Mechanisms for Additive Manufacturing of Conductive Traces

Additive Manufacturing (AM) processes enable the fabrication of miniaturized and flexible devices on complex geometries. This paper explores a hybrid additive manufacturing technology that integrates micro-extrusion and PICO-jetting methods. Conductive slurries and colloidal inks were optimized for their rheological properties to aid their precise deposition. A variety of conductive materials which include carbon, silver, nano-particle silver and nickel were deposited on both rigid (glass) and flexible (Kapton) substrates. The deposited traces were cured using two sintering mechanisms which include furnace heating and in situ laser irradiation. The effect of curing mechanism on the conductance of deposited traces was evaluated. The results indicated that traces could be cured successfully with the laser curing mechanism. Nickel and silver laser cured traces had lower resistivity than the furnace sintered traces. An increase in the laser power resulted in lower resistivity of the traces. The lowest resistivity was achieved at 40W laser power with a single laser pass. Scanning electron microscopy and energy dispersive spectroscopy were used to characterize the trace morphology and elemental compositions. Higher power laser curing resulted in better bonding of the particles. Laser cured samples had minimal oxidation to the cross-section region of the traces as compared to furnace cured samples. Furthermore, this research lays the foundation for the fabrication of electronic components for a high level of freeform 3D electronics using a hybrid additive manufacturing technology.

42 ENGINEERING↗

Blending Polyurethane Thermosets Using Dynamic Urethane Exchange

Recycling crosslinked polyurethanes (PUs) is accomplished through mechanical or chemical processes that are energy-intensive or produce plastics of lesser value. Polymer recycling processes are notably intolerant of polymer mixtures, yet the ability to reprocess and compatibilize two or more crosslinked PUs together will make this process more amenable to mixed waste streams while offering an opportunity to tune the properties of the recycled polymer products. Here, we blend a rigid polyester PU and a soft polyether PU using twin-screw extrusion to yield materials with tunable mechanical properties based on the feed composition. Their material properties were compared to those of compression-molded reprocessed blends and blends where the monomers were mixed prior to synthesis. The extruded materials showed similar mechanical and thermal properties to newly prepared blends and had higher-value mechanical properties compared to the samples reprocessed via compression molding. The morphologies of the blends were observed using phase imaging via atomic force microscopy to show that there is less phase separation in the extruded materials compared to compression-molded blends. The mechanical properties of these materials were tunable from soft to elastomeric to rigid based on the feed composition, and this tunability was demonstrated through four consecutive reprocessing cycles, through which the mechanical properties were steadily varied from rigid to soft by incorporating increasing amounts of soft polyether PU material. Here, this blending method for reprocessing mixed waste compatibilizes different PUs and provides a means to tune the mechanical properties of a PU product, even if starting from waste streams of varying compositions. As such, this process represents an intriguing new approach for polymer reprocessing.

Extrusion↗

Microstructural Evolution of Al-1Fe (Weight Percent) Alloy During Accumulative Continuous Extrusion Forming

As a new microstructure refining method, accumulative continuous extrusion forming (ACEF) cannot only refine metal matrix but also refine the phases that exist in it. In order to detect the refinements of grain and second phase during the process, Al-1Fe (wt pct) alloy was processed by ACEF, and the microstructural evolution was analyzed by electron backscatter diffraction (EBSD) and transmission electron microscopy (TEM). Results revealed that the average grain size of Al-1Fe (wt pct) alloy decreased from 13 to 1.2 μm, and blocky Al{sub 3}Fe phase with an average length of 300 nm was granulated to Al{sub 3}Fe particle with an average diameter of 200 nm, after one pass of ACEF. Refinement of grain was attributed to continuous dynamic recrystallization (CDRX), and the granulation of Al{sub 3}Fe phase included the spheroidization resulting from deformation heat and the fragmentation caused by the coupling effects of strain and thermal effect. The spheroidization worked in almost the entire deformation process, while the fragmentation required strain accumulation. However, fragmentation contributed more than spheroidization. Al{sub 3}Fe particle stimulated the formation of substructure and retarded the migration of recrystallized grain boundary, but the effect of Al{sub 3}Fe phase on refinement of grain could only be determined by the contrastive investigation of Al-1Fe (wt pct) alloy and pure Al.

36 MATERIALS SCIENCE↗

In Situ Electron Microscopy Investigation of Sodiation of Titanium Disulfide Nanoflakes

Two-dimensional (2D) metal sulfides show great promises for their potential applications as electrode materials of sodium ion batteries because of the weak interlayer van der Waals interactions which allow the reversible accommodation and extraction of sodium ions. The sodiation of metal sulfides can undergo a distinct process compared to that of lithiation, which is determined by their metal and structural types. Yet, the structural and morphological evolution during its electrochemical sodiation is still unclear. In this report, we studied the sodiation reaction dynamics of TiS 2 by employing in situ transmission electron microscopy and first-principles calculations. During the sodium ion intercalation process, we observed multiple intermediate phases (phase II, phase Ib, and phase Ia), different from its lithiation counterpart, with varied sodium occupation sites and interlayer stacking sequences. Further insertion of Na ions prompted a multi-step extrusion reaction which led to the phase separation of Ti metal from the Na 2 S matrix, with its 2D morphology expanded to a 3D morphology. In contrast to regular conversion electrodes, TiS 2 still maintained a compacted structure after a full sodiation. Frist-principles calculations reveal that the as-identified phases are thermodynamically preferred at corresponding intercalation/extrusion stages compared to other possible phases. The current work provides the fundamental mechanistic understanding of the sodiation process of 2D transition metal sulfides.

25 ENERGY STORAGE↗

Additive Manufacturing Using Epoxy and Anhydride Curatives

ORNL worked with Dixie Chemical Company to develop epoxy material solutions with anhydride curatives printable on a large-scale printer. Rheological evaluation showed that the addition of high surface area fillers produced a stable yield-stress fluid that is capable of being used in extrusion deposition additive manufacturing. The resulting printed structures have the necessary mechanical and thermomechanical performance to be used in elevated temperature tooling for various composites processing, such as an autoclave.

36 MATERIALS SCIENCE↗

Effects Of Thermal Exchange On Material Flow During Steel Thixoextrusion Process

Semisolid processing is an innovative technology for near net-shape production of components, where the metallic alloys are processed in the semisolid state. Taking advantage of the thixotropic behavior of alloys in the semisolid state, significant progress has been made in semisolid processing. However, the consequences of such behavior on the flow during thixoforming are still not completely understood. To explore and better understand the influence of the different parameters on material flow during thixoextrusion process, thixoextrusion experiments were performed using the low carbon steel C38. The billet was partially melted at high solid fraction. Effects of various process parameters including the initial billet temperature, the temperature of die, the punch speed during process and the presence of a Ceraspray layer at the interface of tool and billet were investigated through experiments and simulation. After analyzing the results thus obtained, it was identified that the aforementioned parameters mainly affect thermal exchanges between die and part. The Ceraspray layer not only plays a lubricant role, but also acts as a thermal barrier at the interface of tool and billet. Furthermore, the thermal effects can affect the material flow which is composed of various distinct zones.

36 MATERIALS SCIENCE↗

Additive Manufacturing of Parts and Tooling in Robotic Systems

ORNL worked with Transcend Robotics, LLC to explore additive manufacturing of the two-piece compression body for their ARTI mobile robot platform. Extrusion compression molding was identified as an effective means of manufacturing these parts. ORNL consulted on modifications to the housing design to accommodate the selected manufacturing process. Parts were printed using ORNL's FDM machines for testing and evaluation of the design as a precursor to molding the parts. The assembly and evaluation of the parts proved favorable and minor design changes to improve assembly and performance were identified.The goal is to develop a light weight and rugged two-part robotic enclosure for an unmanned ground vehicle UGV) that will be used in search and rescue applications. The FDM parts fabricated by ORNL allowed Transcend Robotics to assemble a prototype robot and verify that the new parts will meet the performance requirements. ORNL fabricated enclosure parts out of ABS and Nylon 12 materials such that the design could be tested prior to fabricating tooling for compression molding of Nylon 6 with carbon fiber fill. The robot was performance tested and compared with the previous manufacturing techniques and found to have superior performance.

42 ENGINEERING↗

Unconventional Materials Processing Using Spark Plasma Sintering

Spark plasma sintering (SPS) has gained recognition in the last 20 years for its rapid densification of hard-to-sinter conventional and advanced materials, including metals, ceramics, polymers, and composites. Herein, we describe the unconventional usages of the SPS technique developed in the field. The potential of various new modifications in the SPS technique, from pressureless to the integration of a novel gas quenching system to extrusion, has led to SPS’ evolution into a completely new manufacturing tool. The SPS technique’s modifications have broadened its usability from merely a densification tool to the fabrication of complex-shaped components, advanced functional materials, functionally gradient materials, interconnected materials, and porous filter materials for real-life applications. The broader application achieved by modification of the SPS technique can provide an alternative to conventional powder metallurgy methods as a scalable manufacturing process. The future challenges and opportunities in this emerging research field have also been identified and presented.

36 MATERIALS SCIENCE↗

MODELLING FIBER ORIENTATION DURING ADDITIVE MANUFACTURING COMPRESSION MOLDING PROCESSES

The production of high-performance thermoplastic composites reinforced with short carbon fibers can be achieved by a novel “additive manufacturing-compression molding” technique. An advantage of such combination is two-fold: controlled fiber orientation in additive manufacturing and less void content by compression molding. In this study, a computational fluid dynamics model has been developed to predict the behavior of printed layers during fiber-reinforced thermoplastic extrusion and subsequent compression molding. The fiber orientation was modelled with a simple quadratic closure model. The interaction between the fibers is included using a rotary diffusion coefficient which becomes significant in concentrated regimes. Finally, the second order orientation tensor is coupled with the momentum equation as an anisotropic part of the stress term. The effect of processing parameters on the behavior of printed layers was investigated to determine the favorable printing scenarios. The developed numerical model enables design of high-performance composites with tunable mechanical properties.

Seta, Berin↗

Novel Fabrication of a TiB{sub 2} Grain Refiner and its Effect on Reducing Hot Tearing in AZ91D Magnesium Alloy

Despite the increased use of magnesium (Mg) alloys in diverse engineering applications in recent years, further incorporation of complex Mg alloy castings remains challenging due to the alloy’s relatively high susceptibility to hot tearing. A significant reduction in hot tearing via grain refinement was achieved in aluminum and ferrous alloys; however, an effective, long-lasting and inexpensive grain refiner for aluminum-containing Mg alloys remains elusive. In this work, a TiB{sub 2} grain refiner was fabricated via a novel spark plasma sintering (SPS) powder metallurgy process. Then, its effectiveness in grain refining an AZ91D magnesium alloy was compared to that of a commercially available TiB{sub 2} grain refiner produced by hot extrusion. Due to the homogeneous distribution of the TiAl{sub 3} and TiB{sub 2} particles in the grain refiner, as well as their effect on the alloy’s microstructure evolution and solidification behavior, the SPS-TiB{sub 2} grain refiner was observed to achieve a significant reduction in the grain size and hot tearing of the Al-containing AZ91D magnesium alloy.

36 MATERIALS SCIENCE↗

On the 3D printability of silicone-based adhesives via viscous paste extrusion

Silicone, a commonly used household and construction adhesive, filler, or sealant, is also known for its flexibility, thermal stability, and insulating properties. It is viable as a conformally 3D-printed elastomeric matrix for flexible electronics and biomedical applications. Since most of the popular 3D printing methods use precise print specifications and defined resolution, this study explored the 3D printability of commercial silicone adhesives via a paste extrusion setup. Its viscoelastic and composition properties including the dimensional accuracy and mechanical properties of printed objects using controlled print parameters have been investigated. Finally, these experimental processes in 3D printing should pave the way in using materials originally intended for household use.

36 MATERIALS SCIENCE↗

Fiber orientation effects on ultra-high performance concrete formed by 3D printing

Despite the growing interest in 3D concrete printing, its current progress is limited by reinforcing methods. Inclusion of steel fibers is a potential reinforcing solution; however, the effect of printing process on orientation of the fibers is still unknown. This study aims to quantitatively investigate the orientation distribution of steel fibers in 3D printed ultra-high performance concrete. The effects of extrusion nozzle size, Cartesian print speed, and fiber volume fraction on the orientation of fibers were evaluated using digital image analysis. The consequent effects of the fiber orientation on the mechanical properties of the 3D-printed specimens were also determined. The results were compared with those of the conventionally mold-cast specimens. The results revealed that the smaller nozzle size and higher fiber volume fraction significantly enhanced the fiber alignment parallel to the printing direction. This preferential fiber alignment led to superior mechanical performance of the printed specimens to the mold-cast specimens.

36 MATERIALS SCIENCE↗

Chemical Recycling of Polycaprolactones via Reactive Melt Processing

Chemical recycling is a promising technology for the deconstruction of waste plastics into monomers or other chemical intermediates, which can be converted into other value-added products or repolymerized into polymers. In this work, polycaprolactone and poly(4-propylcaprolactone) were chemically recycled by exploiting ring-closing depolymerization (RCD). To demonstrate the utility of this approach, reactive distillation experiments were initially conducted in a heated round-bottom flask with a distillation head to explore the effect of temperature and catalyst loading on RCD. Inspired by industrial devolatilization equipment, analogous experiments were conducted using a twin-screw melt compounder that was modified to simultaneously heat and mix polymer in the presence of a catalyst while continuously removing the evolved monomer vapors with a vacuum system and collecting them in a cold trap. Yield and selectivity of the recovered monomer were characterized by 1 H nuclear magnetic resonance spectroscopy and gas chromatography-mass spectrometry. Importantly, the more scalable twin-screw melt compounder approach produced values of monomer selectivity (∼90%) and yield (∼80%) similar to those of the round-bottom flask experiments. The recovered monomers were also successfully repolymerized into the same neat polymer with comparable molar masses without purification steps or adding initiator. Here, the results of this study promote the use of reactive devolatilization extrusion as a scalable approach to polyester depolymerization.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

The role of processing route on the microstructure of 14YWT nanostructured ferritic alloy

Nanostructured ferritic alloys (NFAs) have outstanding high temperature creep properties and extreme tolerance to radiation damage. To achieve these properties, NFAs are fabricated by mechanical alloying of metallic and yttria powders. Atom probe tomography has demonstrated that milling times of at least 40 h are required to produce a uniform distribution of solutes in the flakes. After milling and hot extrusion, the microstructure consists of -Fe, high number densities of Ti-Y-O-vacancy-enriched nanoclusters, and coarse Y2Ti2O7 and Ti(O,C,N) precipitates on the grain boundaries. In contrast, the as-cast condition consists of -Fe with 50-100 m irregularly-shaped Y2Ti2O7 pyrochlore precipitates with smaller embedded precipitates with the Al5Y3O12 (yttrium-aluminum garnet) crystal structure indicating that this traditional processing route is not a viable approach to achieve the desired microstructure. The nano-hardnesses were also substantially different, i.e., 4 and 8 GPa for the as-cast and as-extruded conditions, respectively. These differences can be explained by the differences in the microstructure and the effects of the high vacancy content introduced by mechanical alloying, and the strong binding energy of vacancies with O, Ti, and Y atoms retarding diffusion.

36 MATERIALS SCIENCE↗

Ultra-Fine Grain Structures Of Model Al-Mg-Si Alloys Produced By Hydrostatic Extrusion

Microstructure and mechanical properties were studied in model Al-Mg-Si alloys (Al-1 % Mg-0.8% Si and Al-0.5% Mg-0.3% Si-wt %) deformed by hydrostatic extrusion (HE) to strains of 1.4 and 3.8. In these alloys the different percentage of two hardening second-phase precipitates (Mg{sub 2}Si and Si) were observed. The microstructure was characterized by transmission electron microscopy and optical microscopy. The microstructure of the alloys in the initial state was built of coarse grains of an average diameter of {approx}30 rim. The refined microstructure was examined qualitatively and quantitatively using the stereological method and a computer image analysis. The deformation-processed structures evolved very rapidly, forming ultrafine grained (UFG) materials with grains of about 0.4 {mu}m. In addition, the grain refinement in the HE-treated materials has a substantial effect on their properties, such as the mechanical strength and micro-hardness which increase significantly. It has been found that, after {epsilon} = 3.8 in the Al-1% Mg-0.8% Si alloy, the micro-hardness increases approximately twofold. The yield stress is more than four times higher in the UFG alloys, in comparison to the initial state. Similar results were identified in the Al-0.5% Mg-0.3% Si. This is due to the very rapid refinement of the microstructure during the deformation and presence of second-phase particles.

36 MATERIALS SCIENCE↗

Additive Manufacturing of Isotropic NdFeB PPS Bonded Permanent Magnets

Extrusion based additive manufacturing of polymer composite magnets can increase the solid loading volume fraction with greater mechanical force through the printing nozzle as compared to traditional injection molding process. About 63 vol% of isotropic NdFeB magnet powders were compounded with 37 vol% of polyphenylene sulfide and bonded permanent magnets were fabricated while using Big Area Additive Manufacturing without any degradation in magnetic properties. The polyphenylene sulfide bonded magnets have a tensile stress of 20 MPa, almost double than that of nylon bonded permanent magnets. Additively manufactured and surface-protective-resin coated bonded magnets meet the industrial stability criterion of up to 175 °C with a flux-loss of 2.35% over 1000 h. They also exhibit better corrosion resistance behavior when exposed to acidic (pH = 1.35) solution for 24 h and also annealed at 80 °C over 100 h (at 95% relative humidity) over without coated magnets. Thus, polyphenylene sulfide bonded, additively manufactured, protective resin coated bonded permanent magnets provide better thermal, mechanical, and magnetic properties.

36 MATERIALS SCIENCE↗

Processing of non-oxide ceramics from sol-gel methods

A general procedure applied to a variety of sol-gel precursors and solvent systems for preparing and controlling homogeneous dispersions of very small particles within each other. Fine homogenous dispersions processed at elevated temperatures and controlled atmospheres make a ceramic powder to be consolidated into a component by standard commercial means: sinter, hot press, hot isostatic pressing (HIP), hot/cold extrusion, spark plasma sinter (SPS), etc.

36 MATERIALS SCIENCE↗

High Toughness and Fast Crystallization Poly(Lactic Acid)/Polyamide 11/SiO{sub 2} Composites

A poly(lactic acid) (PLA)/polyamide 11 (PA11)/SiO{sub 2} composite was mixed from PLA, PA11, and nanosilica particles through twin-screw extrusion. The PLA/PA11/SiO{sub 2} composite was evaluated with tensile and Izod impact tests, light transmission and haze measurement, and isothermal and nonisothermal crystallization behavior determinations. The PLA/PA11/SiO{sub 2} (97.0/3.0) composite had approximately 10.8% less ultimate tensile strength than neat PLA, but it had greater ductility and approximately ninefold greater elongation at break. A dimple morphology was observed on the fractural surface of the PLA/PA11/SiO{sub 2} composite, indicating that the incorporation of PA11 and nanosilica particles increased the ductility of the PLA matrix. PLA with less than 3 wt% of PA11 and 0.5 phr of nanosilica particles had an Izod impact strength of 8.72 kJ/m{sup 2}. PA11 and nanosilica particles effectively toughened this PLA polymer; they accelerated both isothermal and nonisothermal crystallization rates and increased the crystallinities of the resulting composites under isothermal and nonisothermal crystallization processes.

36 MATERIALS SCIENCE↗