The influence of MgO addition on the densification and microstructure of alumina (Al2O3) was studied. Compacted alumina specimens were manufactured using ball-milling and one-directional pressing followed by sintering at temperatures below 1700oC. Relative density, shrinkage, hardness, and microstructure were investigated using analytical tools such as FE-SEM, EDS, and XRD. When the MgO was added up to 5.0 wt% and sintered at 1500oC and 1600oC, the relative density exhibited an average value of 97% or more at both temperatures. The maximum density of 99.2% was with the addition of 0.5 wt% MgO at 1500oC. Meanwhile, the specimens showed significantly lower density values when sintered at 1400oC than at 1500oC and 1600oC owing to the relatively low sintering temperature. The hardness and shrinkage data also showed a similar trend in the change in density, implying that the addition of approximately 0.5 wt% MgO can promote the densification of Al2O3. Studying the microstructure confirmed the uniformity of the sintered alumina. These results can be used as basic compositional data for the development of MgOcontaining alumina as high-dielectric insulators.
A mixture of elemental Co50Si50 powders was subjected to mechanical alloying (MA) at room temperature to prepare a CoSi thermoelectric compound. Consolidation of the Co50Si50 mechanically alloyed powders was performed in a spark plasma sintering (SPS) machine using graphite dies up to 800 °C and 1,000 °C under 50 MPa. We have revealed that a nanocrystalline CoSi thermoelectric compound can be produced from a mixture of elemental Co50Si50 powders by mechanical alloying after 20 hours. The average grain size estimated from a Hall plot of the CoSi intermetallic compound prepared after 40 hours of MA was 65 nm. The degree of shrinkage of the consolidated samples during SPS became significant at about 450 °C. All of the compact bodies had a high relative density of more than 94 % with a metallic glare on the surface. X-ray diffraction data showed that the SPS compact produced by sintering mechanically alloyed powders for 40-hours up to 800 °C consisted of only nanocrystalline CoSi with a grain size of 110 nm.
In this study, factors considered to be causes of promotion of densification of sintered pellets identified during phase change are reviewed. As a result, conclusions shown below are obtained for each factor. In order for MA powder to soften, a temperature of 1,000 K or higher is required. In order to confirm the temporary increase in density throughout the sintered pellet, the temperature rise due to heat during phase change was found not to have a significant effect. While examining the thermal expansion using the compressed powder, which stopped densification at a temperature below the MA powder itself, and the phase change temperature, no shrinkage phenomenon contributing to the promotion of densification is observed. The two types of powder made of Ti-silicide through heat treatment are densified only in the high temperature region of 1,000 K or more; it can be estimated that this is the effect of fine grain superplasticity. In the densification of the amorphous powder, the dependence of sintering pressure and the rate of temperature increase are shown. It is thought that the specific densification behavior identified during the phase change of the Ti-37.5 mol.%Si composition MA powder reviewed in this study is the result of the acceleration of the powder deformation by the phase change from non-equilibrium phase to equilibrium phase.
This study investigated the densification behavior of rhenium alloys including W-25 wt.%Re and Re-2W-1Ta (pure Re) during sintering. The dilatometry experiments were carried out to obtain the in-situ shrinkage in H2 atmo-sphere. The measured data was analyzed through shrinkage, strain rate and relative density, and then symmetricallytreated to construct the linearized form of master sintering curve (MSC) and MSC as a well-known and straightforwardapproach to describe the densification behavior during sintering. The densification behaviors for each material were ana-lyzed in many respects including apparent activation energy, densification parameter, and densification ratio. MSC witha minimal set of preliminary experiments can make the densification behavior to be characterized and predicted as wellas provide guideline to sinter cycle design. Considering the results of linearized form and MSC, it was confirmed thatthe W-25 wt.%Re compared to Pure Re is more easily densified at the relatively low temperature.
The densification behavior of Al-20Si-5.5Fe-1.2Mg-0.5Mn powders was investigated through micro-structure analysis of sintered specimens. The specimens sintered in vacuum or in high purity (99.999%) nitrogen showed porous near-surface microstructures. The densification of near-surface part was enhanced by means of ultra-high purity (99.9999%) nitrogen atmosphere. The relationship between slow densification and oxide surfaces of Al alloy powders was discussed. And the effects of Mg addition, nitrogen gas, and humidity on densification were discussed. In addition, the rapid growth of primary Si crystals above the critical temperature was reported.
The effect of sintering aids and glass-frit on the densification and resistivity of silver paste was investigated in an effort to enhance the sintered density and electrical conductivity of the silver electrode. To prepare Pb-free silver paste for use at low sintering temperatures, two commercial silver powders (0.8 μm and 1.6 μm in size) and 5wt.% lab-synthesized nanoparticles (30-50 nm in size) as a sintering aids were mixed with 3 wt.% or 6 wt.% of glass frit (Bi2O3-based) using a solvent and three roll mills. Thick films from the silver paste were prepared by means of screen printing on an alumina substrate followed by sintering at 450˚C to 550˚C for 15 min. Silver thick films from the paste with bimodal particles showed a high packing density, high densification during sintering and low resistivity compared to films created using monomodal particles. Silver nanoparticles as a sintering aid enhanced the densification of commercial silver powder at a low sintering temperature and induced low resistivity in the silver thick film. The glass frit also enhanced the densification of the films through liquid phase sintering; however, the optimum content of glass frit is necessary to ensure that a dense microstructure and low resistivity are obtained, as excessive glass-frit can provoke low conductivity due to the interconnection of the glass phase with the high resistivity between the silver particles.
The fabrication of Fe alloy-40 wt.%TiC composite materials using spark plasma sintering process after ball-milling was studied. Raw powders to fabricate Fe alloy-TiC composite were Fe alloy, and activated carbon. Fe alloy powder was Distaloy AE (4%Ni-1%Cu-0.5%Mo-0.01%C-bal.%Fe) made by Hoeganes company with better toughness and lower melting point. These powders were ball-milled in horizontal attrition ball mill at a ball-to-powder weight ratio of 30 : 1. After that, these mixture powders were sintered by using spark plasma sintering apparatus for 5 min at in vacuum atmosphere under torr. DistaloyAE-40 wt.%TiC composite was directly synthesized by dehydrogenation and carburization reaction during sintering process. The phase transformation of as-milled powders and sintered materials was confirmed using X-ray diffraction (XRD) and transmission electron microscope (TEM). The density and harness materials was measured in order to confirm the densification behavior. In case of DistaloyAE-40 wt.%TiC composite retained for 5 min at , it has the relative density of about 96% through the influence of rapid densification and fine TiC particle reinforced Fe-based composites materials.
In all conventional sintered PM products, the pores present are of two types, primary and secondary. Primary pores forming during compaction and latter during sintering, due to penetration of formed liquid through the matrix grain boundary. Effect of carbon addition on diffusion of Cu in SH737-2Cu system was investigated. After compaction and transient liquid phase sintering at and , samples were characterized for densification, showing rise in sintering density and reduction in swelling on carbon addition. Quantitative microstructural characterization (shape factor and pore size) revealed bimodal distribution for 0% carbon, more rounded pores for 0.9% carbon and higher sintering temperature, and pore coarsening at higher sintering temperature.
Nanostructured Alumina - 20 vol% 3YSZ composites powder were synthesized by wet-milling technique. The starting materials were a mixture of Alumina micro-powder and 3YSZ nano-powders. Nano-crystalline grains were obtained after 24 h milling time. The nano-structured powder compacts were then processed to full density at different temperatures by high-frequency induction heat sintering (HFIHS). Effects of temperature on the mechanical and microstructure properties have been studied. composites with higher mechanical properties and small grain size were successfully developed at relatively low temperatures through this technique.
It is known that powder characteristics including particle size and distribution, particle shape, and chemical composition are important parameters which influence direct laser sintering of metal powders. In this paper, we introduce a first order kinetics model for densification of steel powders during laser sintering. A densification coefficient (K) is defined which express the potential of different powders to be laser-sintered to a high density dependent on their particle characteristics.
Both densification and grain growth are driven by the reduction of the interfacial area, kinetics of which depends strongly on the interface structure. Abnormal grain coarsening in the system of singular solid/liquid interface such as WC-Co alloys was explained by the growth mechanism of 2-dimensional nucleation. Based on this concept, the marked inhibition of coarsening of WC grains by VC addition can be approached by the increase in the step free energy, which increases the barrier of 2-dimensional nucleation. The activated sintering in tungsten powders can be approached by the interface structure change induced by the addition of a small amount of nickel.
Mechanically-alloyed NiAl powder was sintered by Spark-Plasma Sintering (SPS) process. Densification and behavior mechanical property were determined from the experimental results and analysis ,such as changes in linear shrinkage, shrinkage rate, microstructure, and phase during sintering process, Victors hardness, and transver.ie-rupture-strength (TRS). Above 97% relative density was obtained after sintering at 115 for 5 min. Crystallite size determined by the Scherrer method was approximately 50 nm. From the X-ray diffraction analysis it was confirmed that the sintered bodies were composed mainly of NiAl phase together with NiAl phase. Measured Vickers hardness and TRS value were 55510 and 139375 MPa , respectively.
Spark-Plasma Sintering(SPS) is one of the new sintering methods which takes advantages both inconventional pressure sintering and electric current sintering. It is known that SPS is very effective for the densification of hard-to-sinter materials like refractory metals, intermetallic compounds, glass and ceramics without grain growth. However, a clear explanation for sintering mechanism and an experimental evidence for the formation of weak plasma during SPS are not given yet. In this study, fundamental study on sintering behavior and mechanism of SPS was investiged. For this study, various spherical Fe powders were prepared such as as-received, as-reduced, and as-oxidized and then sintered by SPS facility. In order to confirm the surface cleaning effect during SPS neck region and fracture surface of sintered body was observed and analyzed by SEM/EPMA. Densification behavior was analyzed from the data of deflection along the pressure axis. Some specimens were additionally produced by Hot Pressing and the results were compared with those of SPS.