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At least 217 records · Page 12

In-Situ X-Ray Diffraction Observations of Low Temperature Ag-Nanoink Sintering and High Temperature Eutectic Reaction with Copper

Nanoinks, which contain nm sized metallic particles suspended in an organic dispersant fluid, are finding numerous microelectronic applications. Nanoinks sinter at much lower temperatures than bulk metals due to their high surface area to volume ratio and small radius of curvature, which reduces their melting points significantly below their bulk values. The unusually low melting and sintering temperatures have unique potential for materials joining since their melting points increase dramatically after initial sintering. In this paper Ag nanoink is studied using in-situ synchrotron based x-ray diffraction to follow the kinetics of the initial sintering step by analysis of diffraction patterns, and to directly observe the high remelt temperature of sintered nanoinks. Ag nanoink is further explored as a possible eutectic bonding medium with copper by tracking phase transformations to high temperatures where melting occurs at the Ag-Cu eutectic temperature, demonstrating nanoinks as a viable eutectic bonding medium.

36 MATERIALS SCIENCE↗

Sintering Kinetics of Inkjet Printed Conductive Silver Lines on Insulating Plastic Substrate

This paper focuses on sintering kinetics of inkjet printed lines containing silver nanoparticles deposited on a plastic substrate. Upon heat treatment, the change of resistance in the printed lines was measured as a function of time and sintering temperatures from 150 to 200 C. A critical temperature was observed for the sintering process, beyond which there was no further reduction in resistance. Analysis shows the critical temperature correlates to the boiling point of the solvent, which is attributed to a liquid-mediated sintering mechanism. It is demonstrated that the sintering process shuts down after the solvent has completely evaporated.

36 MATERIALS SCIENCE↗

An Investigation of the Effect of Sintering Conditions on the Mechanical Behavior of Electroplated Nickel Foams

This study investigates the effect of sintering temperature on the compression strength of nickel foams in an inert atmosphere. The nickel foams were produced by the electrodeposition technique on polyurethane foam substrate. As-plated Ni foams were sintered at 873 K, 1073 K, and 1273 K (600 °C, 800 °C, and 1000 °C) in order to eliminate polyurethane and to enhance ductility at a controlled atmosphere. A compression test was used to determine the mechanical behavior. The morphology of produced foams was analyzed by scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), and X-ray diffraction (XRD) techniques. Quantitative EDS analysis implied that carbon diffuses into nickel structure during the polyurethane decomposition. The amount of carbon in nickel foam increases with heat treatment temperature. The results also reveal that the oxygen impurity arisen from polymer vapors can diffuse into the nickel structure at elevated sintering temperature [i.e., 1273 K (1000 °C)]. The compression curve of as-plated foam showed brittle behavior due to the electroplating condition. The sintering process in the neutral atmosphere could create ductile foams, although the strength of the foams decreases with an increase in the sintering temperature.

36 MATERIALS SCIENCE↗

Thermoelectric Properties of TiNiSn Half Heusler Alloy Obtained by Rapid Solidification and Sintering

Thermoelectric TiNiSn-based half Heusler compound reveals high Seebeck coefficient and electrical conductivity, leading to high power factor. As a consequence of the solidification path, TiNiSn single phase cannot be obtained directly from the liquid phase. Thus, a long annealing step is needed to homogenize the alloy. In this work, we present a new processing route for half Heusler compound formation, combining arc melting of pure elements, rapid solidification of the molten alloy and sintering. Rapid solidification of the molten alloy allows to obtain almost single TiNiSn phase, limiting the formation of the primary TiNi{sub 2}Sn phase as a consequence of the deep undercooling of the liquid. The rapidly solidified alloy was ground to powder and sintered by open die pressing. As-sintered samples show a density around 95% of the theoretical value. Thermal cycling of the sintered samples shows evolution of the phases, suggesting that after sintering the sample is not in equilibrium yet. After the second thermal cycle thermoelectric properties become reproducible, indicating the attainment of the equilibrium. In conclusion, the proposed processing route allows to obtain dense TiNiSn in bulk form avoiding the time-consuming annealing step, typically used to homogenize this alloy after solidification.

36 MATERIALS SCIENCE↗

Microstructure and Properties of Mn-Cu-Based Damping Alloys Prepared by Ball Milling and Hot-Press Sintering

A Mn-Cu-based damping alloy with a nominal composition of 70Mn-24Cu-3Zn-3Al (at.%) was prepared by ball milling of pure elemental powders and subsequent hot-press sintering of powder mixture at 750 and 825 °C for 2 h. For comparison, this alloy was also prepared by induction melting technology and then homogenized at 850 °C for 24 h. Further, they were aged at 430 °C for 2 h. The microstructure, damping capacity and microhardness of the hot-press-sintered and induction-melted alloys have been investigated. The results show that the microstructure of the powder mixture upon ball milling mainly comprises convoluted composite particles containing α-Mn and γ-Cu phases, and isolated α-Mn ones around. The high compactness of the alloys is obtained after hot-press sintering (94.8 and 98.6% at 750 and 825 °C, respectively). At a holding temperature of 750 °C, the microstructure of the alloy is primarily composed of γ-MnCu, γ-CuMn and α-Mn grains. With increasing the target temperature to 825 °C, the single γ-MnCu solid solution has been formed in the alloy by diffusion of Mn etc. into γ-Cu lattices. The hot-press-sintered alloys (especially at 825 °C) possess relatively high damping capacity although which is still lower than that of induction-melted one. In contrast, the microhardness of the hot-press-sintered alloys (especially at 750 °C) is obviously higher than that of the induction-melted one.

36 MATERIALS SCIENCE↗

Predicting Sintering Window of Binder Jet Additively Manufactured Parts Using a Coupled Data Analytics and CALPHAD Approach

Batch-to-batch variation in powder compositions for binder jet additive manufacturing (BJAM) can significantly deter defining an “ideal” sintering window for a given alloy. One way to overcome the problem is by running sintering experiments at various temperatures for each batch of the powder. However, such an approach increases the time required to achieve large-scale production of parts. The predictive capabilities of computational thermodynamic tools like CALPHAD can be leveraged to overcome the challenge, especially for binder jet additive manufacturing, since the process occurs under near-equilibrium conditions. However, calculating the sintering window using CALPHAD can be computationally expensive, considering many possible feedstock compositions within “specification”. Here, we generate high throughput CALPHAD data for nickel-based superalloys to develop machine learning models to predict the sintering window rapidly. The predictive capability of the models has been validated using published results on BJAM of Inconel 718 and 625. Further, validated models are lightweight and can be deployed in an industrial setting to get sintering window in an accelerated manner.

36 MATERIALS SCIENCE↗

Investigation of temperature approximation methods during flash sintering of ZnO

The lattice expansion in ZnO, using in-situ X ray diffraction, has been investigated during flash sintering with varying current densities. While current flow through the specimen enhances the kinetics of sintering for ZnO, the temperature is not high enough to claim thermal runaway or localized melting. Unlike the case of yttria stabilized zirconia [1,2], experimental temperature approximations predict comparable specimen temperature to conventional sintering temperature of ZnO. Microstructural analysis supports the findings of the in-situ temperature approximations. In comparison with black body radiation, a gap between theoretical value and measured value was found due to flaws in the theoretical model. In addition, a new type of flash sintering was introduced, with current ramp, to avoid the power spike which has been the source of much debate about the transition from voltage to current control. In conclusion, the advantage of this method is in the controlled sintering kinetics thus avoiding the channeling found in dielectric materials [3].

36 MATERIALS SCIENCE↗

Grand potential sintering simulations of doped UO 2 accident-tolerant fuel concepts

Chromium-doped UO is a widely-studied near-term deployable accident-tolerant fuel concept because it results in a dense, large-grain structure that increases the fuel resistance to densification, swelling, and fission gas release. A new charged-interstitial mechanism was recently proposed to describe the behavior of dopants like chromium in sintered UO 2 . Based on that mechanism, manganese was suggested as an even stronger dopant than chromium. In the current work we use mesoscale sintering simulations in an effort to validate the new mechanism. We compare the relative behavior of Cr-doped and undoped UO 2 against experimental data in the literature. We also make predictions of the relative behavior of Mn-doped UO 2 . Simulations are done using the phase field-based grand potential sintering model. Dopants have two effects on sintered UO 2 . They marginally increase the densification rate and greatly increase the average grain size. Both of these effects are individually tested in small-scale simulations. Then large 3D sintering simulations are used to test the combined behavior of both effects. The results for the densification rate simulations are consistent with experiments for Cr-doped fuels. However, we note the grain growth rates are lower than what is found in the literature for Cr-doped fuels.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Physical and hydraulic properties of modern sinter deposits: El Tatio, Atacama

We report sinters are siliceous, sedimentary deposits that form in geothermal areas. Formation occurs in two steps. Hot water circulates in the subsurface and dissolves silica from the host rock, usually rhyolites. Silica then precipitates after hot water is discharged and cools. Extensive sinter formations are linked to up-flow areas of fluids originating from high temperature (> 175 °C) deep reservoirs. Fluid geochemistry, microbial communities, and environmental conditions of deposition determine the texture of sinter and pore framework. Porosity strongly influences physical and hydraulic properties of rocks. To better understand the properties controlling the transport of fluids, and interpret geophysical observations in geothermal systems, here we studied 17 samples of modern geyserite sinter deposits (< 10 ka) from the active El Tatio geothermal field in northern Chile. We measured the physical properties (hydraulic, seismic, and electrical), and internal microstructure (using μX-Ray computed tomography). We find that the pore structure, and thus hydraulic and physical properties, is controlled by the distribution of microbial matter. Based on velocity-porosity relationships, permeability-porosity scaling, and image analysis of the 3D pore structure; we find that the physical and hydraulic properties of sinter more closely resemble those of vesicular volcanic rocks and other material formed by precipitation in geothermal settings (i.e., travertine) than clastic sedimentary rocks.

15 GEOTHERMAL ENERGY↗

Effects of sintering aid CuTa{sub 2}O{sub 6} on piezoelectric and dielectric properties of sodium potassium niobate ceramics

Graphical abstract: NKN ceramics with a sintering aid CuTa{sub 2}O{sub 6} (CT) doping increased the mechanical quality factor (Q{sub m}) and electromechanical coupling factor (k{sub p}). Highlights: Black-Right-Pointing-Pointer A new sintering aid CuTa{sub 2}O{sub 6} was developed to dope into NKN ceramics. Black-Right-Pointing-Pointer Dense NKN ceramics were obtained as CuTa{sub 2}O{sub 6} compound doping. Black-Right-Pointing-Pointer We find the soluble limit of CuTa{sub 2}O{sub 6} compound incorporated into NKN ceramics. Black-Right-Pointing-Pointer The maximum Q{sub m} and k{sub p} values were more than 1500 and 42%, respectively. Black-Right-Pointing-Pointer CuTa{sub 2}O{sub 6} compound is a better sintering aid compared with K{sub 5.3}Cu{sub 1.3}Ta{sub 10}O{sub 29}. -- Abstract: In this study, the effects of a sintering aid CuTa{sub 2}O{sub 6} (CT) on (Na{sub 0.5}K{sub 0.5})NbO{sub 3} (NKN) ceramics were investigated. The diffracted angles in XRD profiles decreased because the Nb-sites were replaced by Cu and Ta ions, causing the expansion of lattice volume. SEM images showed smaller grain sizes at a low concentration of CuTa{sub 2}O{sub 6}, and grain sizes increased as the concentration of CuTa{sub 2}O{sub 6} doping increased because of a liquid phase formed. When CuTa{sub 2}O{sub 6} dopants were doped into NKN ceramics, the T{sub O-T} and T{sub c} phase transitions decreased because the replacement of Ta{sup 5+} ions in the B-site. A high bulk density (4.595 g/cm{sup 3}) and electromechanical coupling factor (k{sub p}, k{sub t}) were enhanced when CT dopants were doped into NKN ceramics. Moreover, the mechanical quality factor (Q{sub m}) also increased from 67 to 1550. NKN ceramics with sintering aid CuTa{sub 2}O{sub 6} doping showed excellent piezoelectric properties: k{sub p}: 42.5%; k{sub t}: 49.1%; Q{sub m}: 1550; and d{sub 33}: 96 pC/N.

36 MATERIALS SCIENCE↗

Structure, sintering behavior, and microwave dielectric properties of (1 − x) CaWO{sub 4}–xYLiF{sub 4} (0.02 ≤ x ≤ 0.10) ceramics

Highlights: • Structure, sinterability, and dielectric properties of CaWO{sub 4}–YLiF{sub 4} were studied. • CaWO{sub 4} can be densified (TD 97%) at 750 °C/2 h by YLiF{sub 4} doping. • Excellent microwave dielectric properties could be obtained. - Abstract: Structures and sintering behaviors of (1 − x) CaWO{sub 4}–xYLiF{sub 4} (0.02 ≤ x ≤ 0.10) ceramic have been investigated by X-ray powder diffraction (XRD), dilatometry, scanning electron microscopy (SEM) in this work. The microwave dielectric properties were measured with a network analyzer at the frequency of about 8–15 GHz. Limited solid solution could be formed within the compositional range of x < 0.1. The sintering temperature of CaWO{sub 4} could successfully be reduced to ∼750 °C/2 h by doping with small amount of YLiF{sub 4}. An optimized microwave dielectric properties with ϵ{sub r} = 10.5, Q × f = 73 000 GHz and τ{sub f} = −37.7 ppm/°C could be obtained after sintered at the 750 °C for 2 h for x = 0.04 compositions. XRD and back scattering SEM analysis indicated that the (1 − x) CaWO{sub 4}–xYLiF{sub 4} (x = 0.04) ceramic could be chemically compatible with Ag after sintering at 750 °C/2 h.

36 MATERIALS SCIENCE↗

Magnetic and electrical properties of Z-type hexaferrites sintered in different atmospheres

Graphical abstract: Oxygen atmosphere played an important role in inhibiting electrons hopping between Fe{sup 2+} and Fe{sup 3+} and reducing both of magnetic and dielectric losses of Ba{sub 3}Co{sub 2}Fe{sub 24}O{sub 41}, which is favorable in view of antenna substrate applications. - Highlights: • Co{sub 2}Z-type hexaferrites were sintered in different atmospheres. • The losses of the sample sintered in O{sub 2} were reduced effectively without additive. • A 3RC equivalent circuit model was put forward in the impedance analysis. - Abstract: Co{sub 2}Z-type hexaferrites with stoichiometric composition of Ba{sub 3}Co{sub 2}Fe{sub 24}O{sub 41} were fabricated by using a conventional solid–state reaction method. The influence of sintering atmosphere, namely air, O{sub 2} and N{sub 2}, on magnetic and electrical properties of the hexaferrites was systematically investigated. This work reveals that O{sub 2} played an important role in inhibiting the formation of Fe{sup 2+} and thus reducing magnetic and dielectric losses. The Co{sub 2}Z specimen sintered at 1300 °C in O{sub 2} atmosphere showed promising magneto-dielectric properties. Specifically, the magnetic and dielectric losses were less than 0.05 and 0.005 in the frequency range of 30–300 MHz, respectively. Impedance spectra were performed to reveal the underlying mechanisms for the different electrical properties of the Co{sub 2}Z ceramics sintered in different atmospheres.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Sintering behaviors, phases, and dielectric properties of MO-TeO2-V2O5 (M = Ca, Sr, Ba) ultralow temperature ceramics

Highlights: • Introduction of TeO{sub 2} to MO-V{sub 2}O{sub 5} (M = Ca,Sr,Ba) ceramics promoted a M{sub 2}V{sub 2}O{sub 7} phase formation, and obtain excellent dielectric properties and a densification sintering at below 600°. • Chemical compatibility of ULTCC ceramics with aluminum electrode indicated that aluminum did not react with MO-TeO{sub 2}-V{sub 2}O{sub 5} ceramics. • Aluminum easily encouraged the transformation of M{sub 2}V{sub 2}O{sub 7} structures to M{sub 3}(VO{sub 4}){sub 2} structures and other structures under the ultra-low temperature sintering. - Abstract: Influences of TeO{sub 2} on phase evolutions and sintering behaviors of MO-TeO{sub 2}-V{sub 2}O{sub 5} (M = Ca, Sr, Ba) ultralow temperature ceramics were investigated using X-ray diffraction (XRD) and scanning electron microscopy (SEM). Dielectric properties of MO-TeO{sub 2}-V{sub 2}O{sub 5} (M = Ca, Sr, Ba) ceramics and their chemical compatibility with an aluminum electrode were also studied. Introducing TeO{sub 2} to MO-V{sub 2}O{sub 5} (M = Ca, Sr, Ba) ceramics obviously decreased the sintering temperature and promoted formation of M{sub 2}V{sub 2}O{sub 7} (M = Ca, Sr, Ba) phases. Also, dielectric properties mainly depend on the amount of TeO{sub 2} added to MO-TeO{sub 2}-V{sub 2}O{sub 5} ceramics. Investigation of chemical compatibility with aluminum shows that aluminum does not react chemically with MO-TeO{sub 2}-V{sub 2}O{sub 5} ceramics; however, aluminum causes transformation of M{sub 2}V{sub 2}O{sub 7} phases to other phases (such as M{sub 3}(VO{sub 4}){sub 2}) to be easier. Sintering temperature of MO-TeO{sub 2}-V{sub 2}O{sub 5} (M = Ca, Sr, Ba) ceramics can be regulated below 600 °C, which is much less than the melting point of aluminum. In addition, MO-TeO{sub 2}-V{sub 2}O{sub 5} (M = Ca, Ba) ceramics maintain quality factors of ∼18,000 GHZ, a dielectric constant of 10–12, and dielectric loss lower than 10{sup −4}.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Anisotropic lattice expansion determined during flash sintering of BiFeO 3 by in-situ energy-dispersive X-ray diffraction

BiFeO 3 has a Curie temperature (T C ) of 825 °C, making it difficult to sinter with conventional methods while maintaining the purity of the material, as unavoidably secondary phases appear at temperatures above T c . Flash sintering is a relatively new technique that saves time and energy compared to other sintering methods. BiFeO 3 was flash sintered at 500 °C to achieve 90% densification. In-situ energy dispersive X-ray diffraction (EDXRD) reflected that the material did not undergo any phase transformation, having been sintered well below the T C . Interestingly, anisotropic lattice expansion in the materialwas observed when the sample was exposed to the electric field.

36 MATERIALS SCIENCE↗

Studying the sintering behavior of BeO{sub x}-SiC{sub 1-x} Composite ceramic Material

The sintering behavior for BeO-SiC compacts composite ceramic at different sintering temperatures in air were conducted, resulting data indicated that the percentage of SiC (Wt% 5) sintered at 800 C deg. lead to higher sintering density of (1.80 gm/cm3). The x-ray diffraction pattern analysis indicated nothing change concerning the crystal structure. Microstructure development has been studied as a function SiC content. Silicon carbide found to be suppressed the sinter ability of the matrix BeO powder.

36 MATERIALS SCIENCE↗

Nanocrystallization in spark plasma sintered Fe{sub 48}Cr{sub 15}Mo{sub 14}Y{sub 2}C{sub 15}B{sub 6} bulk amorphous alloy

Spark plasma sintering (SPS) is evolving as an attractive process for the processing of multi-component Fe-based bulk amorphous alloys and their in-situ nanocomposites with controlled primary nanocrystallization. Extended Q-range small angle neutron scattering (EQ-SANS) analysis, complemented by x-ray diffraction and transmission electron microscopy, was performed to characterize nanocrystallization behavior of SPS sintered Fe-based bulk amorphous alloys. The SANS experiments show significant scattering for the samples sintered in the supercooled region indicating local structural/compositional changes associated with the profuse nucleation of nanoclusters (∼4 nm). For the samples spark plasma sintered near and above crystallization temperature (>653 °C), the SANS data show the formation of interference maximum indicating the formation and growth of (Fe,Cr){sub 23}C{sub 6} crystallites. The SANS data also indicate the evolution of bimodal crystallite distribution at higher sintering temperatures (above T{sub x1}). The growth of primary nanocrystallites results in impingement of concentration gradient fields (soft impingement effect), leading to non-random nucleation of crystallites near the primary crystallization.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Effect of TiO{sub 2} additives to the sintering of Y{sub 2}O{sub 3}

The effect of sintering additive on the microstructure development of yttrium oxide was investigated. Different combinations of yttrium oxide with TiO{sub 2} were used as x-ray diffraction, differential thermal analysis (DTA) were sintering additive. The investigated and microstructure of resulting compacts were characterized by, using scanning electron microscopy, porosity and sintering density for all compacting samples sintered at different sintering temperature under static air.

36 MATERIALS SCIENCE↗

Improvement of mechanical properties by additive assisted laser sintering of PEEK

The additive assisted laser sintering was recently developed at IKT: A carbon black (CB) additive is used to adjust the polymer's laser absorption behavior with the aim to improve the interconnection of sintered powder layers. In this paper a parameter study, Polyetheretherketone (PEEK) samples were prepared with different contents of carbon black and were laser sintered with varying thermal treatment. The samples were mechanically tested and investigated by optical light and transmission electron microscopy. An influence on the morphology at the border areas of particles and intersections of laser sintered layers was found. Depending on the viscosity of the raw material and CB content, different shapes of lamellae were observed. These (trans-) crystalline or polymorph structures, respectively, influence the thermal and mechanical behavior of the virgin PEEK. Moreover, the thermal treatment during the sintering process caused an improvement of mechanical properties like tensile strength and elongation at break.

36 MATERIALS SCIENCE↗