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At least 397 records · Page 22

Internal defect detection and characterization of samarium-cobalt sintered magnets by ultrasonic testing technique

Excessive quantities of samarium-cobalt (Sm-Co) magnet material are being scrapped needlessly due to a lack of understanding of inhomogeneity distribution and unacceptable internal defects. If there is a way to identify, locate, characterize and when needed separate the defective portions of magnet material, utilization can be increased and product quality improved. Further, the magnets’ magnetic and mechanical performance can be improved by reducing the occurrence of internal defects. This paper reports on a cost-effective and efficient nondestructive evaluation method based on an ultrasonic testing (UT) technique applied for detecting and characterizing internal defects in Sm-Co sintered magnets. Applying the UT technique will allow users to comprehensively analyze internal defects, such as inclusions, porosity, microcracks, and other structural irregularities, check for homogeneity and anomalous regions and give the locations of these internal anomalies and defects within the Sm-Co sintered magnets. The UT technique can also be applied to other rare-earth permanent magnets, such as sintered or die-upset neodymium-iron-boron (Nd-Fe-B) magnets. The UT technique can effectively guide quality control and acceptable product selection, in addition to optimizing the magnet alloy design and production processes. Therefore, it can facilitate the improvement of magnet manufacturing efficiency and machinability, reduce scrap, prolong service life, increase the use of what would be post-production waste, and enhance product reuse and recycling at end-of-life disposition.

36 MATERIALS SCIENCE↗

Effect of phosphorus additions on the sintering and transport properties of proton conducting BaZr{sub 0.85}Y{sub 0.15}O{sub 3-{delta}}

The influence of phosphorous additions on the sintering and electrical transport properties of the proton-conducting perovskite BaZr{sub 0.85}Y{sub 0.15}O{sub 3-{delta}} (BZY) has been studied with a view to the use of phosphates as typical dispersants for the formation of stabilised solid suspensions or as possible sintering aids. P{sub 2}O{sub 5} additions, (1-x)BZY{center_dot}xP{sub 2}O{sub 5}, monotonously promote densification in the intermediate compositional range 0.04{<=}x{<=}0.08. Nonetheless, BZY reacts with phosphorous forming the phase Ba{sub 3}(PO{sub 4}){sub 2} at temperatures as low as 600 Degree-Sign C. The associated loss of Ba from the perovskite, leads to a decrease in the perovskite lattice parameter, the formation of yttria-based impurity phases and impaired grain growth. Such reaction has an extremely detrimental effect on bulk and grain boundary conductivities. It is, therefore, vital that the current results are taken into account by the protonics community when attempting to prepare the stabilised solid suspensions of BZY nanopowders required for thin ceramic applications. Alternative dispersants to phosphate esters must be found. - Graphical Abstract: Sintering experiments performed at 1500 Degree-Sign C for 5 h and at 1400 Degree-Sign C for 24 h of (1-x)BaZr{sub 0.85}Y{sub 0.15}O{sub 3-{delta}}{center_dot}xP{sub 2}O{sub 5} in the range x=0-0.10. Highlights: Black-Right-Pointing-Pointer P{sub 2}O{sub 5} additions, (1-x)BZY{center_dot}xP{sub 2}O{sub 5}, promote densification in the intermediate compositional range 0.04{<=}x{<=}0.08. Black-Right-Pointing-Pointer BZY reacts with phosphorous forming the phase Ba{sub 3}(PO{sub 4}){sub 2} at temperatures as low as 600 Degree-Sign C. Black-Right-Pointing-Pointer Detrimental effects on bulk and grain boundary conductivities are shown. Black-Right-Pointing-Pointer Alternative dispersants to phosphate esters must be found.

36 MATERIALS SCIENCE↗

Gallium composition dependence of crystallographic and thermoelectric properties in polycrystalline type-I Ba{sub 8}Ga{sub x}Si{sub 46-x} (nominal x=14-18) clathrates prepared by combining arc melting and spark plasma sintering methods

The gallium composition dependence of crystallographic and thermoelectric properties in polycrystalline n-type Ba{sub 8}Ga{sub x}Si{sub 46-x} (nominal x=14-18) compounds with the type-I clathrate structure is presented. Samples were prepared by combining arc melting and spark plasma sintering methods. Powder x-ray diffraction, Rietveld analysis, scanning electron microscopy, and energy-dispersive x-ray spectroscopy show that the solubility limit of gallium in the type-I clathrate phase is close to x=15, which is slightly higher than that for a single crystal. The carrier concentration at room temperature decreases from 2 Multiplication-Sign 10{sup 21} cm{sup -3} to 4 Multiplication-Sign 10{sup 20} cm{sup -3} as the Ga content x increases. The Seebeck coefficient, the electrical conductivity, and the thermal conductivity vary systematically with the carrier concentration when the Ga content x varies. The effective mass (2.0m{sub 0}), the carrier mobility (10 cm{sup 2} V{sup -1} s{sup -1}), and the lattice thermal conductivity (1.1 W m{sup -1} K{sup -1}) are determined for the Ga content x=14.51. The dimensionless thermoelectric figure of merit ZT is about 0.55 at 900 K for the Ga content x=14.51. The calculation of ZT using the experimentally determined material parameters predicts ZT=0.8 (900 K) at the optimum carrier concentration of about 2 Multiplication-Sign 10{sup 20} cm{sup -3}. - Graphical abstract: The gallium composition dependence of crystallographic and thermoelectric properties is presented on polycrystalline n-type Ba{sub 8}Ga{sub x}Si{sub 46-x} with the type-I clathrate structure prepared by combining arc melting and spark plasma sintering methods. The thermoelectric figure of merit ZT reaches 0.55 at 900 K due to the increase in the Ga content (close to x=15), and a calculation predicts further improvement of ZT at the optimized carrier concentration. Highlights: Black-Right-Pointing-Pointer Crystallographic properties of Ba{sub 8}Ga{sub x}Si{sub 46-x} clathrates are characterized. Black-Right-Pointing-Pointer Arc melting and spark plasma sintering process enables increase of Ga content. Black-Right-Pointing-Pointer We elucidate the Ga composition dependence of thermoelectric properties. Black-Right-Pointing-Pointer Thermoelectric figure of merit ZT is improved due to the increased Ga content. Black-Right-Pointing-Pointer Calculation predicts a potential ZT=0.8 at 900 K at optimized carrier concentration.

36 MATERIALS SCIENCE↗

Evaluation of suitable porosity for sintered porous {beta}-tricalcium phosphate as a bone substitute

Structural and mechanical characterization is performed for sintered porous beta tricalcium phosphate ({beta}-TCP) to determine the appropriate porosity for use as a bone substitute. Four different types of porous {beta}-TCP specimen with different porosities are fabricated through a sintering process. For structural characterization, scanning electron microscopy and a Microfocus X-ray computed tomography system are used to investigate the pore openings on the specimen's surface, pore size, pore distribution, and pore interconnections. Compression tests of the specimens are performed, and mechanical properties such as the elastic modulus and compressive strength are obtained. Also, the geometric shape and volume of the {beta}-TCP around the contact region of two pores, which need to be initially resolved after implantation in order to increase the size of the pore openings, are evaluated through simple calculations. The results show that porous {beta}-TCP with 42.1% porosity may be a suitable bone substitute candidate in terms of sustaining external loads, and inducing and cultivating bone cells. - Highlights: Black-Right-Pointing-Pointer Structural and mechanical characterization was performed for sintered porous {beta}-TCP specimens. Black-Right-Pointing-Pointer For structural characterization, SEM and Microfocus X-ray CT system were used. Black-Right-Pointing-Pointer For mechanical characterization, compression tests were performed. Black-Right-Pointing-Pointer Porous {beta}-TCP with 42.1% porosity may be a suitable bone substitute.

36 MATERIALS SCIENCE↗

The effect of Si on the microstructure and mechanical properties of spark plasma sintered boron carbide

Highlights: • Si addition leads to a dense final product at a low sintering temperature. • The added Si preferentially formed SiC and borosilicate glass instead of replacing the chain atoms in boron carbide. • The hardness of our Si-containing boron carbide is 30–35% greater than currently in-use commercial boron carbide plates. - Abstract: Fully dense boron carbide discs were achieved by spark plasma sintering boron carbide powders with 10 wt% silicon. The silicon did not diffuse into boron carbide grains to produce a solid solution of Si-doped boron carbide; instead the silicon reacted with impurities in the starting powder to form β-SiC and borosilicate glass. The resultant new phases facilitated densification of the multiphase ceramic through liquid phase-assisted sintering. The resultant material exhibits improved hardness (34.3 GPa Vikers hardness under 1 kg load) with toughness comparable to both Si-free and commercially available boron carbide.

36 MATERIALS SCIENCE↗

Phase evolution during spark plasma sintering of novel Si3N4-doped TiB2–SiC composite

Highlights: • The effect of Si{sub 3}N{sub 4} addition on microstructure of TiB{sub 2}–SiC composite was studied. • Fully dense TiB{sub 2}-based composite was obtained by addition of SiC and Si{sub 3}N{sub 4}. • TiC, B{sub 4}C and SiO{sub 2} were formed in Si{sub 3}N{sub 4}-free and Si{sub 3}N{sub 4}-doped TiB{sub 2}–SiC ceramics. • TiN and BN were in-situ formed only in Si{sub 3}N{sub 4}-doped TiB{sub 2}–SiC sample. - Abstract: Spark plasma sintering process was employed to fabricate TiB{sub 2}–SiC and novel Si{sub 3}N{sub 4}-doped TiB{sub 2}–SiC ceramic composites at 1900 °C for 7 min under 40 MPa. The microstructural development of TiB{sub 2}-based composites was significantly influenced by the addition of SiC as a reinforcement phase and Si{sub 3}N{sub 4} as a sintering aid. Thermodynamic assessment, X-ray diffractometry, scanning electron microscopy and energy dispersive spectroscopy disclosed the in-situ formation of TiC, B{sub 4}C and SiO{sub 2} in both samples as well as TiN and BN in the Si{sub 3}N{sub 4}-doped TiB{sub 2}–SiC sample through the chemical reactions of SiC and Si{sub 3}N{sub 4} additives with the surface oxide impurities of TiB{sub 2} particles (TiO{sub 2} and B{sub 2}O{sub 3}). The elimination of harmful oxide layers and the in-situ formation various secondary phases had remarkable influences on the sinterability and final microstructure of TiB{sub 2}.

36 MATERIALS SCIENCE↗

On the Arrhenius-like behavior of conductivity during flash sintering of 3 mol% yttria stabilized zirconia ceramics

Here, we discuss the Arrhenius behavior of electrical conductivity σ during flash sintering of 3 mol% yttria stabilized zirconia (3YSZ). In situ x-ray diffraction is used to determine sample temperature. Sintering contribution to σ is excluded by investigating the flash event on a dense ceramic. We show that total conductivity follows an Arrhenius-like equation in both dense and green samples, even during Stage II of flash. The non-linearity often verified during flash sintering of 3YSZ is therefore related to the furnace temperature instead of the sample temperature when building the ln(σ) vs. 1/T plots. Furthermore, we verified a change in the activation energy for conduction prior to the ignition of the flash event and discussed the possible mechanisms. For instance, the decrease in activation energy from Stage I to II in the dense sample is attributed to a contribution from electronic carriers.

36 MATERIALS SCIENCE↗

Ultrafast Reactive Laser Sintering of Highly Conductive Garnet-Type LLZTO Solid Electrolytes

Rapid and scalable fabrication of garnet-type solid electrolytes remains a major challenge for the practical deployment of lithium metal batteries. Here, we report reactive laser sintering (RLS) as an ultrafast and potentially scalable strategy for fabricating garnet-type Li 6.4 La 3 Zr 1.4 Ta 0.6 O 12 (LLZTO) solid electrolytes. RLS of LLZTO enables simultaneous reaction and densification, achieving ∼95% relative density while minimizing lithium loss and suppressing secondary phase formation. Compared to conventional furnace sintering, RLS promotes enhanced grain growth and improved densification, leading to improved ionic conductivity (0.36 ± 0.08 mS cm −1 ) while maintaining comparable activation energies for Li + transport. Structural characterization by X-ray diffraction (XRD), Raman spectroscopy, and solid-state 6 Li/ 7 Li NMR confirms the formation of cubic garnet LLZTO with homogeneous microscale elemental distribution. In addition, nanoindentation measurements demonstrate that RLS preserves the mechanical properties of the garnet framework despite ultrafast localized thermal processing. By integrating simultaneous reaction and densification with tunable microstructural control, reactive laser sintering provides a promising manufacturing pathway for high-performance garnet solid electrolytes toward next-generation solid-state batteries.

CO2 laser↗

Surface Self-Diffusion Induced Sintering of Nanoparticles

Despite the critical role of sintering phenomena in constraining the long-term durability of nanosized particles, a clear understanding of nanoparticle sintering has remained elusive due to the challenges in atomically tracking the neck initiation and discerning different mechanisms. Through the integration of in situ transmission electron microscopy and atomistic modeling, this study uncovers the atomic dynamics governing the neck initiation of Pt–Fe nanoparticles via a surface self-diffusion process, allowing for coalescence without significant particle movement. Real-time imaging reveals that thermally activated surface morphology changes in individual nanoparticles induce significant surface self-diffusion. Further, the kinetic entrapment of self-diffusing atoms in the gaps between closely spaced nanoparticles leads to the nucleation and growth of atomic layers for neck formation. This surface self-diffusion-driven sintering process is activated at a relatively lower temperature compared to the classic Ostwald ripening and particle migration and coalescence processes. The fundamental insights have practical implications for manipulating the morphology, size distribution, and stability of nanostructures by leveraging surface self-diffusion processes.

36 MATERIALS SCIENCE↗

Intrinsic and extrinsic relaxation of CaCu{sub 3}Ti{sub 4}O{sub 12} ceramics: Effect of sintering

The effect of sintering process on the electrical properties of CaCu{sub 3}Ti{sub 4}O{sub 12} (CCTO) ceramic dielectrics were investigated in this paper. It was found that grain size is affected by sintering and the nonlinear current-voltage (I-V) property will decrease with the increased sintering time. Also, the frequency and temperature dependences of dielectric permittivity and loss in the ranges of 10{sup -1}-10{sup 7} Hz and 130-270 K were studied. Two relaxation processes with activation energy of 0.51 eV and 0.10 eV, respectively, were found in the frequency dependence of tan {delta} and Cole-Cole planes, which can be interpreted in terms of insulating grain boundaries and semiconducting grains. It was suggested that grain boundary Maxwell-Wagner relaxation and ionization of oxygen vacancy V{sub O}{sup ++}, proposed as extrinsic and intrinsic relaxations, are responsible for the dielectric behaviors of CCTO ceramics.

36 MATERIALS SCIENCE↗

Effect of Sintering Temperature on Dielectric Properties of Iron Deficient Nickel-Ferrite

Nickel Ferrite among all the magneto ceramic materials have been studied very much due to its large number of applications. But there is a large scope of modification of its properties. Thus people still working on it for improvisation of its properties via compositional and structural modifications. Present paper reporting the preparation and characterization of iron deficient Nickel ferrite for different sintering temperature. Ferrite samples having the general formula NiFe1.98O{sub 4} were prepared using the standard ceramic method. The phase formation was confirmed by X-ray diffraction technique. The effect of sintering temperature on the electrical properties and resistivity was studied. The data shows that dielectric properties are highly dependent on the sintering temperature.

36 MATERIALS SCIENCE↗

The effects of applied current on one-dimensional interdiffusion between copper and nickel in spark plasma sintering

Spark plasma sintering (SPS) is a powder metallurgy technique that employs the use of fast sintering kinetics to produce final consolidated components in a matter of minutes. In order to use blended powders in SPS to obtain fully alloyed parts, diffusion during sintering must be understood. An investigation into the effects of current on the diffusion of copper and nickel was performed using SPS. Bulk specimens were used to generate diffusion couples in SPS in alternating orientations with respect to the direction of the current. Control samples were produced using a horizontal insertion vacuum furnace. Experiments were performed at temperatures between 850°C and 1000°C for 3 h. Concentration profiles were obtained by the use of both energy-dispersive spectroscopy and a Monte Carlo simulated correction curve. Diffusion coefficients and activation energies were calculated for samples produced by SPS and annealing without current. It was shown that, at temperatures near 0.9 T{sub m}, the application of current in SPS inhibits diffusion between copper and nickel due to the re-orientation of electrons caused by the loss of ferromagnetism in nickel. Activation energy for diffusion is, however, decreased due to the temperature gradients arising from the difference in resistivity between the two species.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Effect of the light spectrum of various substrates for inkjet printed conductive structures sintered with intense pulsed light

In this work, the novel method of intense pulsed light (IPL) sintering of a nanoparticle silver ink is presented. Various patterns are printed with the Inkjet technology on two flexible foils with different light spectra. One is a clear Polyethylenterephthalat [PET] foil and the second is a light brownish Polyimide [PI] foil. The samples are flashed with different parameters regarding to pulse intensity and pulse length. Microscopic images are indicating the impact of the flashing parameters and the different light spectra of the substrates on the sintered structures. Sheet and line resistance are measured and the conductivity is calculated. A high influence of the property of the substrate with respect to light absorption and thermal conductivity on the functionality of printed conductive structures could be presented. With this new method of IPL sintering, highly conductive inkjet printed silver patterns could be manufactured within milliseconds on flexible polymeric foils without damaging the substrate.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Grain refinement in heavy rare earth element-free sintered Nd–Fe–B magnets by addition of a small amount of molybdenum

We employed a modified refractory-metal-addition method to achieve higher coercivity and remanence in heavy rare earth element (HREE)-free Nd–Fe–B sintered magnets. This process involved inducing the formation of a homogeneous secondary phase at the grain boundaries during sintering, making it possible to control the intergrain diffusion by adding small amounts of Mo, a refractory metal. To control the microstructure of the secondary phase effectively, a metal organic compound of the refractory metal was coated on the surfaces of the particles of an HREE-free Nd–Fe–B powder. The average grain size after this process was 5.60 μm, which was approximately 1.8 μm smaller than that of the HREE-free sintered Nd–Fe–B magnets (7.4 μm). The coercivity of the magnets prepared through this process could be increased from 11.88 kOe to 13.91 kOe without decreasing their remanence.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Effect of sintering on electrical properties of yttrium doped Li-based NASICON compounds

Electrical properties of Lithium based Li{sub 1.3}Al{sub 0.3-x}Y{sub x}Ti{sub 1.7}(PO{sub 4}){sub 3} (LAYTP) system was prepared using solid state reaction route. The samples were subjected to differing duration of sintering. X-ray diffraction was used to investigate the microstructure while density measurement was performed to determine the effect of sintering on the density of the prepared samples. Electrical properties of the material were studied using impedance spectroscopy, in frequency range 20 MHz to 1 Hz and in temperature range 303 K to 423 K. It was found that sample with least amount of yttrium and which was sintered for least duration had superior conductivity over other samples. It was also found that grain boundary conductivity improved marginally for sample with higher proportion of yttrium heat treated for longer duration.

36 MATERIALS SCIENCE↗

Effect of sintering temperatures and screen printing types on TiO{sub 2} layers in DSSC applications

Dye-Sensitized Solar Cell (DSSC) is a candidate solar cell, which has a big potential in the future due to its eco-friendly material. This research is conducted to study the effect of sintering temperature and the type of screen-printing toward the characteristics of TiO{sub 2} layer as a working electrode in DSSC. TiO{sub 2} layers were fabricated using a screen-printing method with a mesh size of T-49, T-55, and T-61. TiO{sub 2} layers were sintered at temperatures of 600°C and 650°C for 60 min. DSSC structure was composed of TiO{sub 2} as semiconductors, ruthenium complex as dyes, and carbon as counter electrodes. The morphology of TiO{sub 2} layer was observed by using Nikon E2 Digital Camera Microscopy. The efficiencies of DSSC were calculated from the I-V curves. The highest efficiency is 0.015% at TiO{sub 2} layer fabricated with screen type T-61 and at a sintering temperature of 650°C.

14 SOLAR ENERGY↗

Sintering time effect on crystal structure and magnetic properties of Bi{sub 0.8}La{sub 0.2}FeO{sub 3} multiferroics

Effect of sintering time over the structure and magnetic properties has been studied in Bi{sub 0.8}La{sub 0.2}FeO{sub 3} multiferroic ceramics prepared by solid state reaction technique. The structure changes with the advent mixed phase rhombohedral and orthorhombic symmetry to immaculate orthorhombic structure with sintering time from 2 to 3 hour, as revealed by means of the simulation of XRD patterns via Rietveld analysis through FullProf software. The M – H plots depict decent enhancement in magnetization with values of remnant magnetization (Mr) from 0.01868emu/g to 0.09357emu/g while the sintering time is varied from 2 to 3 hour. The metamagnetic transition may be attributed to the crumpling of the modulated spin cycloid existing inherently in the pristine compound. The presented study may have considerable impact in commercial as well as advanced electronic applications.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Effect of sintering treatment on structural and magnetic properties of Ni{sub 0.5}Co{sub 0.5}Fe{sub 2}O{sub 4} ferrites

Two sets of Ni{sub 0.5}Co{sub 0.5}Fe{sub 2}O{sub 4} ferrites were synthesized using sol-gel method. Both the samples were heat treated at different temperatures. The effect of sintering treatment analyzed on structural and magnetic properties. X-ray diffraction (XRD) and scanning electron microscope (SEM) were used for structural analysis. Alternating gradient magnetometer (AGM) is used for magnetic measurements. In structural analysis, grains size is calculated using Debye - Scherrer’s formula and Williamson-Hall (W-H) plot. From both the techniques, grain size is found nearly same and increased in size with increase sintering temperature. Increased particle size is confirmed from SEM micrographs. Strain value is calculated from intercept of W-H plot. In both the samples, compressive strain in nature is found. Magnetic properties were also varying under different heat treatment. The change in magnetic properties with change in structural change at different sintering treatment is discussed in this report.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗