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At least 325 records · Page 18

Unveiling 3D Morphology of Multiscale Micro-Nanosilver Sintering for Advanced Electronics Manufacturing by Ptychographic X-ray Nanotomography

The sintering processing–structure–property relationship of a multiscale silver materials is investigated: microparticles with nanofeatures, particularly on their three-dimensional (3D) morphology. The target application is to replace conventional lead-based solders in advanced electronic manufacturing. Unlike lead-based solders, silver powders are suited to satisfy increasingly demanding mechanical, electrical, and thermal requirements, meanwhile being free of health effect. Sintering the material at a low temperature and without applied pressure are desirable conditions, which results in a preferred use of silver nanoparticles, as nanofeatures have higher driving force to sinter with the decrease in particle size. However, nanosized powders present potential health/environmental effects. To address the trade-off between the benefits and shortcomings of nano-versus microparticles, this work studies a novel multiscale silver paste, namely micron-sized powders with nanosized features. To get quantitative 3D visualization of micro- and nanoscale features, ptychographic X-ray computed nanotomography is applied. The correlations between conditions (thermal aging, pressure, and substrate metallization), mechanical properties, and morphological parameters are established. Finally, using novel 3D X-ray nanoimaging technique, it is demonstrated that one can design multiscale materials while balancing complex demands required in advanced electronics manufacturing and research directions in materials design and characterization.

36 MATERIALS SCIENCE↗

Thick Binder-Free Electrodes for Li-Ion Battery Fabricated Using Templating Approach and Spark Plasma Sintering Reveals High Areal Capacity

The templating approach is a powerful method for preparing porous electrodes with interconnected well-controlled pore sizes and morphologies. The optimization of the pore architecture design facilitates electrolyte penetration and provides a rapid diffusion path for lithium ions, which becomes even more crucial for thick porous electrodes. In this work, NaCl microsize particles are used as a templating agent for the fabrication of 1 mm thick porous LiFePO 4 and Li 4 Ti 5 O 12 composite electrodes using spark plasma sintering technique. These sintered binder-free electrodes are self-supported and present a large porosity (40%) with relatively uniform pores. The electrochemical performances of half and full batteries reveal a remarkable specific areal capacity (20 mA h cm -2 ), which is 4 times higher than those of 100 µm thick electrodes present in conventional tape-casted Li–ion batteries (5 mA h cm -2 ). The 3D morphological study is carried out using full field transmission X-ray microscopy in microcomputed tomography mode to obtain tortuosity values and pore size distributions leading to a strong correlation with their electrochemical properties. These results also demonstrate that the coupling between the salt templating method and the spark plasma sintering technique turns out to be a promising way to fabricate thick electrodes with high energy density.

25 ENERGY STORAGE↗

Bioinspired Nacre‐Like Alumina with a Metallic Nickel Compliant Phase Fabricated by Spark‐Plasma Sintering

Abstract Many natural materials present an ideal “recipe” for the development of future damage‐tolerant lightweight structural materials. One notable example is the brick‐and‐mortar structure of nacre, found in mollusk shells, which produces high‐toughness, bioinspired ceramics using polymeric mortars as a compliant phase. Theoretical modeling has predicted that use of metallic mortars could lead to even higher damage‐tolerance in these materials, although it is difficult to melt‐infiltrate metals into ceramic scaffolds as they cannot readily wet ceramics. To avoid this problem, an alternative (“bottom‐up”) approach to synthesize “nacre‐like” ceramics containing a small fraction of nickel mortar is developed. These materials are fabricated using nickel‐coated alumina platelets that are aligned using slip‐casting and rapidly sintered using spark‐plasma sintering. Dewetting of the nickel mortar during sintering is prevented by using NiO‐coated as well as Ni‐coated platelets. As a result, a “nacre‐like” alumina ceramic displaying a resistance‐curve toughness up to ≈16 MPa m ½ with a flexural strength of ≈300 MPa is produced.

Wat, Amy↗

Cantilever testing of sintered-silver interconnects

Cantilever testing is an underutilized test method from which results and interpretations promote greater understanding of the tensile and shear failure responses of interconnects, metallizations, or bonded joints. The use and analysis of this method were pursued through the mechanical testing of sintered-silver interconnects that joined Ni/Au-plated copper pillars or Ti/Ni/Ag-plated silicon pillars to Ag-plated direct bonded copper substrates. Sintered-silver was chosen as the interconnect test medium because of its high electrical and thermal conductivities and high-temperature capability—attractive characteristics for a candidate interconnect in power electronic components and other devices. Deep beam theory was used to improve upon the estimations of the tensile and shear stresses calculated from classical beam theory. The failure stresses of the sintered-silver interconnects were observed to be dependent on test-condition and test-material-system. In conclusion, the experimental simplicity of cantilever testing, and the ability to analytically calculate tensile and shear stresses at failure, result in it being an attractive mechanical test method to evaluate the failure response of interconnects.

36 MATERIALS SCIENCE↗

Effect of the Ce Content on the Magnetic Properties and Microstructure of CeCo{sub 5}-based Sintered Bulk Magnets

CeCo{sub 5}-based magnets have recently attracted much attention due to their moderate magnetic performance and low cost. Nevertheless, there have been few studies on the effects of Ce content on the magnetic properties and microstructures of CeCo{sub 5}-based magnets. In response to this, the magnetic properties of sintered bulk magnets with nominal compositions of Ce(Co{sub 0.73}Cu{sub 0.135}Fe{sub 0.135}){sub z} (z = 4.95, 5.15, 5.35, and 5.55), prepared by the conventional powder metallurgy method, were investigated here. Based on experimental findings, it was shown that Ce(Co{sub 0.73}Cu{sub 0.135}Fe{sub 0.135}){sub 5.15} sintered bulk magnets had comprehensive magnetic properties—maximum energy product of 80 kJ m{sup − 3} (10 MGOe) and intrinsic coercivity (H{sub cj}) of 452 kA m{sup − 1} (5.69 kOe)—superior to those previously reported by us. For z = 5.35 and 5.55, due to the presence of the minor Ce{sub 2}Co{sub 17} phase (which has a Curie temperature (T{sub c}) < 20 °C), magnets had low H{sub cj} values. Based on x-ray diffraction and scanning electron microscopy observations, it was suggested that the volume fraction of the 1:5 matrix phase was the main factor determining the H{sub cj} of CeCo{sub 5}-based sintered bulk magnets obtained with different Ce contents. Furthermore, the importance of the dispersion characteristics of the Ce{sub 2}O{sub 3} phase within the matrix was emphasized. Uniform dispersion of the Ce{sub 2}O{sub 3} phase can significantly improve the overall magnetic performance of CeCo{sub 5}-based magnets.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Effects of Post-sintering Annealing on (NdLa)-(FeCo)-B Magnets

A common limitation of La substitutions into (Nd, La) 2 Fe 14 B magnets is the reduction of the anisotropy field (H a ), which decreases magnet coercivity (H cj ). In this study, adding a small amount of Pr-Cu to a La-containing neo magnet may modify the grain boundary (GB), which can help recover a fraction of the degraded H cj . An optimal GB modification requires a carefully designed post-sinter heat treatment, which is the focus of this work on characterizing the effects of multi-step post-sintering annealing on the evolutions of microstructure and magnetic properties. We find that Nd and Cu concentrations at GBs and triple junctions (TJs) increase when the annealing temperatures are lowered. Annealing temperatures of 580°C and 480°C (near rare-earth-rich eutectic temperatures) enabled the development of a thick and continuous GB phase, which helps to magnetically decouple the grains, and, thus, enhance H cj . For the alloy with 25% Nd replaced by La, and with the addition of 7.5 wt.% of Pr 68 Cu 32 as GB modifier, the optimized multi-step post-sinter annealing improved the H cj from 4.8 kOe to 9 kOe.

36 MATERIALS SCIENCE↗

Review of Solid State Consolidation Processing Techniques of ODS Steels (Hot Extrusion, Hot Isostatic Pressing, Spark Plasma Sintering, and Stir Friction Consolidation): Resulting Microstructures and Mechanical Properties

This paper reviews the solid-state consolidation processing techniques for Oxide Dispersion Strengthened steels and compares them in terms of the resulting microstructure and reported mechanical properties. Synthesis techniques include hot extrusion, hot isostatic pressing, spark plasma sintering and friction consolidation. The effects of process parameters on the resulting microstructures and performance are discussed for each technique. Average oxide size, average grain size, and porosity are compared across techniques, as well as mechanical strength and ductility. Across consolidation techniques where temperature can be controlled, a low sintering temperature with a high sintering pressure is favorable for keeping oxide sizes, grain sizes, and porosity low. The use of yttrium and titanium for oxide formation has been evidenced to reduce oxide sizes, and tungsten additions have been shown to improve strength. Current literature suggests that the more mature hot extrusion technique produces stronger steel with consistently fine oxides, while other alternative solid-state consolidation, while promising, offer margin for improvement.

36 MATERIALS SCIENCE↗

Combined DSC/TGA Analysis to Rationalize the As-Sintered Microstructure in Binder Jet Additively Manufactured H13 Tool Steel

In this study, a combined DSC/TGA analysis has been used to rationalize the constant liquid channel width at higher sintering temperatures in H13 tool steel manufactured by binder jet additive manufacturing. Using enthalpy conservation along with coupled DSC + TGA analysis, the phase fractions of liquid and austenite phases during heating and cooling respectively were estimated. The estimates from the DSC/TGA analysis were compared with equilibrium phase fraction predictions from ThermoCalc. The resulting phase evolution was correlated to the as-sintered microstructure to rationalize the unexpected lack of change in liquid channel width at higher sintering temperatures.

Kannan, Rangasayee↗

Evolution of the nanoporous microstructure of sintered Ag at high temperature using in-situ X-ray nanotomography

Silver pastes sintering is a potential candidate for die bonding in power electronic modules. The joints, obtained by sintering, exhibit a significant pore fraction, thus reducing the density of the material compared to bulk silver. The mechanical properties (Young's modulus, yield strength and ultimate tensile stress) are then drastically altered. However, while careful analysis of the nanoporous structure has been reported in 2D, little is known about its quantitative spatial evolution during thermal aging and more specifically during temperature jumps endured by the assembly during operation. High temperature evolutions of the 3D nanoporous structure have been observed in-situ using a heater fitted into the beamline 6-2c at SLAC-SSRL. Segmentation of the porosity and subsequent statistical analysis of the tomographic dataset reveal a complex evolution of the porous nanostructure including growth, separation and coalescence at a constant density. Such an analysis provides insight into the microstructural evolution of sintered nanoporous Ag joints in-service.

36 MATERIALS SCIENCE↗

Laser pre-sintering for denudation reduction in the laser powder bed fusion additive manufacturing of Ti-6Al-4V alloy

As a fundamentally different process for creation of complex parts, laser powder bed fusion (LPBF) additive manufacturing exhibits complex behavior at the melt pool that has a direct influence on the macroscopic properties of the final material. Powder denudation, a previously studied deleterious phenomenon, is the displacement of powder due to entrainment in a jet of rapidly vaporized metal created by the process laser. To minimize the effect of denudation and inspired by methods in adjacent fields, a laser pre-sintering (LPS) method was studied in an effort to reduce denudation. LPS was found to be most effective in the 1–4 J/mm3 volumetric energy density processing regimes, minimizing the common experimentally observed problems with the LPBF process. Scanning electron microscopy of the LPS-treated powder bed revealed insight into the accelerating effect morphological irregularities along the powder particle surface have in the pre-sintering process. To further understand the process, an estimation of the sintered neck sizes necessary to eliminate denudation in LPS is made, qualitatively affirming the low energy densities needed to prevent denudation. Here, the results presented in this work represent an initial step towards understanding and implementing LPS as a quality-enhancing step in LPBF.

36 MATERIALS SCIENCE↗

Perovskite evolution on La modified Mn 1.5 Co 1.5 O 4 spinel through thermal ageing with enhanced oxidation activity: Is sintering always an issue?

Non-precious metal oxides have great potential in catalytic deep oxidation of emitted hydrocarbons to help address various environmental pollution concerns. However, sintering issue is a stumbling block in practical application upon long-term high-temperature operation or thermal shock experience. Herein, La was applied to modify Mn 1.5 Co 1.5 O 4 spinel to get a highly active oxidation catalyst with exceptional stability against high-temperature thermal ageing treatment. With thermal ageing at 750 °C for 100 h, the La modified Mn–Co composite reached 90 % conversion in toluene oxidation at 265 °C under the high WHSV of 120,000 mL g -1 h -1 , while this value increased to 312 °C over blank Mn–Co spinel. The addition of La not only inhibited the growth of spinel nanocrystals, but also brought about perovskite formation through sintering, generating perovskite-spinel interfaces, thus enhancing both activity and stability. Meanwhile, the La modified Mn–Co spinel exhibited superior performance in presence of water or sulfur dioxide after thermal ageing treatment. In conclusion, this work offers a versatile strategy to design anti-sintering and active oxidation nanocatalysts based on non-precious metal oxides for industrial applications.

36 MATERIALS SCIENCE↗

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

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

01 COAL, LIGNITE, AND PEAT↗

Consolidation of Molybdenum nanopowders by spark plasma sintering: Densification mechanism and first mirror application

Mo nanopowders are synthesized by ball milling and the following hydrogen reduction of MoO 3 powders. The densification mechanism of Mo nanopowders during spark plasma sintering (SPS) is analyzed by the combination of the regression of the experimental data on regular SPS and on the SPS multistep pressure dilatometry based on the continuum theory of the sintering. The Mo mirror with 400 nm average grain size and 93% relative density is fabricated by the SPS. The performance of the mirrors made from a single crystal Mo and from the hydrogen-reduced sintered Mo nanopowder is discussed. The microstructure and optical properties of the mirrors are characterized before and after plasma exposure, and no substantial degradation of the reflectivity was observed.

36 MATERIALS SCIENCE↗

Investigation of UO 2 doped with Fe 2 O 3 sintered under a reducing atmosphere

Nuclear fuel produced with trace amounts of transition metal additives is of potential interest for introducing intentional signatures for accelerating nuclear forensics. In this work, we investigate the effects on microstructure, grain size, crystal structure, and stoichiometry when trace amounts of Fe in the form of Fe 2 O 3 are added to UO 2 . Sintering of compacts with different concentrations, from 250 to 3000 ppmw, was performed under a reducing atmosphere at 1773 K. The persistence of the taggant during the fuel fabrication process as well as its impact on grain size, crystal lattice, and first-neighbor chemistry was evaluated using inductively coupled plasma–optical emission spectroscopy, powder X-ray diffraction (pXRD), Raman spectroscopy, scanning electron microscopy–backscatter electron spectroscopy, energy dispersive spectroscopy, and thermogravimetric analysis. We observed that a negligible amount of Fe was lost during sintering. Our results indicate that the feedstock, Fe 2 O 3 transforms into Fe and FeO under the test sintering conditions. For all compositions, metallic Fe precipitate was found in grain boundaries as a secondary phase. In conclusion, the potential incorporation of ionic Fe into the UO 2 unit cell was determined by pXRD and Raman spectra.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Development of nano-Y2O3 dispersed Zr alloys synthesized by mechanical alloying and consolidated by pulse plasma sintering

Highlights: • Zr-Fe-Cr-Cu-Ti-1.0wt% nano-Y{sub 2}O{sub 3} dispersed alloys are fabricated by mechanical alloying and pulse plasma sintering. • These alloys record extremely high compressive strength, Young’s modulus, and hardness. • These mechanical properties are superior as compared to other commercially available Zr based alloys. • Dispersion of nanometric FeZr{sub 2}, Y{sub 2}Ti{sub 2}O{sub 7}, Fe{sub 2}Ti, ZrCu, Cr{sub 2}Zr, Y{sub 2}O{sub 3} leads to grain boundary pinning at elevated temperature. - Abstract: In this paper, Zr alloys are synthesized with nominal compositions: 50Zr-30Fe-10Cr-5Cu-5Ti (alloy A), and 49Zr-30Fe-10Cr-5Cu-5Ti-1Y{sub 2}O{sub 3} (alloy B), 45Zr-30Fe-10Cr-10Cu-5Ti (alloy C), 44Zr-30Fe-10Cr-10Cu-5Ti-1Y{sub 2}O{sub 3} (alloy D) (all in wt%) by mechanical alloying and consolidated by pulse plasma sintering at 1173 K (900 °C), 1223 K (950 °C) and 1273 K (1000 °C) using 75 MPa uniaxial pressure applied for 5 min and 70 kA pulsed current at 3 Hz pulse frequency. The microstructure and phase evolution during mechanical alloying and sintering has been characterized by X-ray diffraction (XRD), scanning and transmission electron microscopy (SEM & TEM) and energy dispersive spectroscopy (EDS). Mechanical properties i.e. hardness and compressive strength were determined by using nano-indentation unit and universal testing machine. The produced alloys recorded very high levels of compressive strength (1359–2456 MPa), and hardness (7.05–10.05 GPa) which measures 1.5–2.0 times more than that of other Zr alloys (2 O{sub 3}) particles which can contribute to grain boundary pinning, and improved creep and oxidation resistance at elevated temperature.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Crystallization Mechanism in Spark Plasma Sintered Bulk Metallic Glass Analyzed using Small Angle Neutron Scattering

Understanding the thermal stability of metallic glasses is critical to determining their safe temperatures of service. In this paper, the crystallization mechanism in spark plasma sintered Fe 48 Cr 15 Mo 14 Y 2 C15B6 metallic glass is established by analyzing the crystal size distribution using x-ray diffraction, transmission electron microscopy and in-situ small angle neutron scattering. Isothermal annealing at 700 °C and 725 °C for 100 min resulted in the formation of (Fe,Cr) 23 C 6 crystals, measured from transmission electron micrographs, to be from 10 to 30 nm. The small angle neutron scattering intensity measured in-situ, over a Q-range of 0.02 to 0.3 Å -1 , during isothermal annealing of the sintered samples, confirmed the presence of (Fe,Cr) 23 C 6 crystals. The measured scattering intensity, fitted by the maximum entropy model, over the Q-range of 0.02 to 0.06 Å -1 , revealed that the crystals had radii ranging from 3 to 18 nm. The total volume fraction of crystals were estimated to be 0.13 and 0.22 upon isothermal annealing at 700 °C and 725 °C for 100 min respectively. The mechanism of crystallization in this spark plasma sintered iron based metallic glass was established to be from pre-existing nuclei as confirmed by Avrami exponents of 0.25 ± 0.01 and 0.39 ± 0.01 at the aforesaid temperatures.

42 ENGINEERING↗

Rheology improvement for silicon nitride and resin slurries for vat photopolymerization printing and sintering

This work presents the formulation, rheological characterization, and sintering of silicon nitride (Si₃N₄) slurries for vat photopolymerization (VPP) using digital light processing (DLP). Bimodal Si₃N₄ powder was dispersed into commercial photopolymer resin using two different dispersants with opposing effects on surface charge, resulting in varied slurry stability and flow behavior. Slurries were engineered to exhibit shear-thinning behavior suitable for VPP, and their flow properties were quantified using a power-law fluid model. The formulations achieved cure depths of approximately 40 µm and enabled printing of green bodies. Post-processing included thermal debinding and liquid-phase sintering, yielding primarily β-Si₃N₄ with a minor Y-Si-Al-O-N glass phase. The sintered parts reached ~85% of theoretical density and demonstrated a flexural strength of ~330 MPa. Microstructural analysis revealed closed porosity along with some defects related to powder agglomeration and interlayer adhesion. These findings provide insights into slurry formulation strategies for additive manufacturing of high-performance non-oxide ceramics.

Aerospace engineering↗

Onset of selective laser flash sintering of AlN

Abstract Flash sintering uses a combination of heating and electric fields to rapidly densify ceramics. Previously, it has been shown that a scanning laser can be used to initiate flash sintering in localized regions on an yttria‐stabilized zirconia (YSZ) sample in a process known as selective laser flash sintering (SLFS). In this work, we show using a combination of measurements of electric current flowing through the sample and observations of necks formed between powder particles that aluminum nitride (AlN) can also undergo SLFS. Scan conditions required to initiate SLFS are characterized over a range of laser powers and laser scan speeds in a dry nitrogen environment. It is shown that initiation of SLFS in AlN is governed by both the local input energy density per scan and heat dissipation and a numerical model is developed to predict temperatures during SLFS. Assuming the minimum temperature along the conductive path determines the onset of SLFS, the minimum temperature and time required is 450–670 K in 2–0.25 s for the pressed AlN pellets used in this study for laser scan speeds of 33–300 m/s, laser powers of 10–30 W, and an applied electric field of 3000 V/cm.

Gouws, Andre↗