Pore Formation Process of Porous Ti3SiC2 Fabricated by Reactive Sintering.
ABSTRACT: Porous Ti3SiC2 was fabricated with high purity, 99.4 vol %, through reactive sintering of titanium hydride (TiH2), silicon (Si) and graphite (C) elemental powders. The reaction procedures and the pore structure evolution during the sintering process were systematically studied by X-ray diffraction (XRD) and scanning electron microscope (SEM). Our results show that the formation of Ti3SiC2 from TiH2/Si/C powders experienced the following steps: firstly, TiH2 decomposed into Ti; secondly, TiC and Ti5Si3 intermediate phases were generated; finally, Ti3SiC2 was produced through the reaction of TiC, Ti5Si3 and Si. The pores formed in the synthesis procedure of porous Ti3SiC2 ceramics are derived from the following aspects: interstitial pores left during the pressing procedure; pores formed because of the TiH2 decomposition; pores formed through the reactions between Ti and Si and Ti and C powders; and the pores produced accompanying the final phase synthesized during the high temperature sintering process.
Project description:This paper presents selected characteristics of the metallic porous materials produced by the sintering of metal powders. The authors focus on materials produced from the iron powder (Fe) of ASC 100.29 and Distaloy SE. ASC 100.29 is formed by atomization and has a characteristic morphology. It consists of spherical particles of different sizes forming agglomerates. Distaloy SE is also based on the sponge-iron. The porous material is prepared using the patented method of sintering the mixture of iron powder ASC 100.29, Fe(III) oxide, Distaloy SE and Fe(III) oxide in the reducing atmosphere of dissociated ammonia. As a result, the materials with open pores of micrometer sizes are obtained. The pores are formed between iron particles bonded by diffusion bridges. The modelling of porous materials containing diffusion bridges that allows for three-dimensional (3D) imaging is presented.
Project description:Fabrication of metallic foams by sintering metal powders mixed with thermally degradable compounds is of interest for numerous applications. Compounds releasing gaseous nitrogen, minimizing interactions between the formed gases and metallic foam by diluting other combustion products, were applied. Cysteine and phenylalanine, were used as gas releasing agents during the sintering of elemental Fe and Al powders in order to obtain metallic foams. Characterization was carried out by optical microscopy with image analysis, scanning electron microscopy with energy dispersive spectroscopy, and gas permeability tests. Porosity of the foams was up to 42 ± 3% and 46 ± 2% for sintering conducted with 5 wt % cysteine and phenylalanine, respectively. Chemical analyses of the formed foams revealed that the oxygen content was below 0.14 wt % and the carbon content was below 0.3 wt %. Therefore, no brittle phases could be formed that would spoil the mechanical stability of the FeAl intermetallic foams. The gas permeability tests revealed that only the foams formed in the presence of cysteine have enough interconnections between the pores, thanks to the improved air flow through the porous materials. The foams formed with cysteine can be applied as filters and industrial catalysts.
Project description:In this study, minor-addition elements such as Si, Co, Cr, W, Mo, and Ti were added to matrix to improve the wettability between the diamonds and Cu matrix. The pressureless liquid-phase sintering technique adopted in this study provides a low-cost method for producing diamond/Cu composites with high potential for industrial mass production. Thermal properties of the diamond/Cu-Ti composites fabricated by pressureless liquid-phase sintering at 1373 K with variation in Ti contents were thoroughly investigated. XRD and TEM analysis show that TiC layer formed in the interface between Cu and diamond. The composites exhibited thermal conductivity as high as 620 W/m · K for 50 vol% diamond/Cu-0.6 at % Ti composite with diamond particle size of 300 µm. This value comes up to 85% of the thermal conductivity calculated by the Hasselman and Johnson (H-J) theoretical analysis. Under these conditions, a suitable coefficient of thermal expansion of 6.9 ppm/K was obtained.
Project description:In situ grown C0.3N0.7Ti and SiC, which derived from non-oxide additives Ti3SiC2, are proposed to densify silicon nitride (Si3N4) ceramics with enhanced mechanical performance via hot-press sintering. Remarkable increase of density from 79.20% to 95.48% could be achieved for Si3N4 ceramics with 5 vol.% Ti3SiC2 when sintered at 1600 °C. As expected, higher sintering temperature 1700 °C could further promote densification of Si3N4 ceramics filled with Ti3SiC2. The capillarity of decomposed Si from Ti3SiC2, and in situ reaction between nonstoichiometric TiCx and Si3N4 were believed to be responsible for densification of Si3N4 ceramics. An obvious enhancement of flexural strength and fracture toughness for Si3N4 with x vol.% Ti3SiC2 (x = 1~20) ceramics was observed. The maximum flexural strength of 795 MPa for Si3N4 composites with 5 vol.% Ti3SiC2 and maximum fracture toughness of 6.97 MPa·m1/2 for Si3N4 composites with 20 vol.% Ti3SiC2 are achieved via hot-press sintering at 1700 °C. Pull out of elongated Si3N4 grains, crack bridging, crack branching and crack deflection were demonstrated to dominate enhance fracture toughness of Si3N4 composites.
Project description:Meso-porous metal materials have enhanced surface energies offering unique surface properties with potential applications in chemical catalysis, molecular sensing and selective separation. In this paper, commercial 20 nm diameter metal nano-particles, including silver and copper were blended with 7 nm silica nano-particles by shear mixing. The resulted powders were cold-sintered to form dense, hybrid thin films. The sacrificial silica template was then removed by selective etching in 12 wt% hydrofluoric acid solutions for 15 min to reveal a purely metallic meso-porous thin film material. The impact of the initial silica nano-particle diameter (7-20 nm) as well as the sintering pressure (5-20 ton·m<sup>-2</sup>) and etching conditions on the morphology and properties of the final nano-porous thin films were investigated by porometry, pyknometery, gas and liquid permeation and electron microscopy. Furthermore, the morphology of the pores and particle aggregation during shear mixing were assessed through cross-sectioning by focus ion beam milling. It is demonstrated that meso-pores ranging between 50 and 320 nm in average diameter and porosities up to 47% can be successfully formed for the range of materials tested.
Project description:Melting metallurgy is still the most frequently used and simplest method for the processing of metallic materials. Some of the materials (especially intermetallics) are very difficult to prepare by this method due to the high melting points, poor fluidity, or formation of cracks and pores after casting. This article describes the processing of Ti-Al-Si alloys by arc melting, and shows the microstructure, phase composition, hardness, fracture toughness, and compression tests of these alloys. These results are compared with the same alloys prepared by powder metallurgy by the means of a combination of mechanical alloying and spark plasma sintering. Ti-Al-Si alloys processed by melting metallurgy are characterized by a very coarse structure with central porosity. The phase composition is formed by titanium aluminides and titanium silicides, which are full of cracks. Ti-Al-Si alloys processed by the powder metallurgy route have a relatively homogeneous fine-grained structure with higher hardness. However, these alloys are very brittle. On the other hand, the fracture toughness of arc-melted samples is immeasurable using Palmqvist's method because the crack is stopped by a large area of titanium aluminide matrix.
Project description:The sintering of metal powders is an efficient and versatile technique to fabricate porous metal elements such as filters, diffusers, and membranes. Neck formation between particles is, however, critical to tune the porosity and optimize mass transfer in order to minimize the densification process. In this work, macro-porous stainless steel (SS) hollow-fibers (HFs) were fabricated by the extrusion and sintering of a dope comprised, for the first time, of a bimodal mixture of SS powders. The SS particles of different sizes and shapes were mixed to increase the neck formation between the particles and control the densification process of the structure during sintering. The sintered HFs from particles of two different sizes were shown to be more mechanically stable at lower sintering temperature due to the increased neck area of the small particles sintered to the large ones. In addition, the sintered HFs made from particles of 10 and 44 ?m showed a smaller average pore size (<1 ?m) as compared to the micron-size pores of sintered HFs made from particles of 10 ?m only and those of 10 and 20 ?m. The novel HFs could be used in a range of applications, from filtration modules to electrochemical membrane reactors.
Project description:In this paper, experimental verification of the microstructural evolution model during sintering of aluminum, iron and particulate mullite ceramic powders using self-propagated high-temperature synthesis (SHS) was performed. The powder mixture with 20% wt. content of reinforcing ceramic was investigated throughout this research. The mixed powders were cold pressed and sintered in a vacuum at 1030 °C. The SHS reaction between sintered feed powders resulted in a rapid temperature increase from the heat generated. The temperature increase led to the melting of an aluminum-based metallic liquid. The metallic liquid infiltrated the porous SiO2 ceramics. Silicon atoms were transited into the intermetallic iron-aluminum matrix. Subsequently, a ternary matrix from the Fe-Al-Si system was formed, and synthesis of the oxygen and aluminum occurred. Synthesis of both these elements resulted in formation of new, fine Al2O3 precipitates in the volume of matrix. The proposed microstructural evolution model for growth of ultra-fine Al2O3 oxides from SiO2 silica ceramic decomposition during SHS was successfully verified through scanning electron microscopy (SEM), X-ray energy-dispersive spectroscopy (EDS) analysis and X-ray diffraction (XRD).
Project description:(Ti,Zr)C powder was sintered with WC-Co following an industrial process, including an isotherm at 1410 °C. A series of interrupted sintering trials was performed with the aim of studying the sintering behavior and the microstructural evolution during both solid-state and liquid-state sintering. Reference samples, using the same elemental compositions but with the starting components TiC and ZrC instead of (Ti,Zr)C, were also sintered. The microstructure was investigated using scanning electron microscopy and energy dispersive X-ray spectroscopy. It is found that the (Ti,Zr)C phase decomposes into Ti-rich and Zr-rich nano-scale lamellae before the liquid-state of the sintering initiates. The final microstructure consists of the binder and WC as well as two different γ phases, rich in either Ti (γ₁) or Zr (γ₂). The γ₂ phase grains have a core-shell structure with a (Ti,Zr)C core following the full sintering cycle. The major differences observed in (Ti,Zr)C with respect to the reference samples after the full sintering cycle were the referred core-shell structure and the carbide grain sizes; additionally, the microstructural evolution during sintering differs. The grain size of carbides (WC, γ₁, and γ₂) is about 10% smaller in WC-(Ti,Zr)C-Co than WC-TiC-ZrC-Co. The shrinkage behavior and hardness of both composites are reported and discussed.
Project description:The WxTaTiVCr high-entropy alloy with 32at.% of tungsten (W) and its derivative alloys with 42 to 90at.% of W with in-situ TiC were prepared via the mixing of elemental W, Ta, Ti, V and Cr powders followed by spark plasma sintering for the development of reduced-activation alloys for fusion plasma-facing materials. Characterization of the sintered samples revealed a BCC lattice and a multi-phase structure. The selected-area diffraction patterns confirmed the formation of TiC in the high-entropy alloy and its derivative alloys. It revealed the development of C15 (cubic) Laves phases as well in alloys with 71 to 90at.% W. A mechanical examination of the samples revealed a more than twofold improvement in the hardness and strength due to solid-solution strengthening and dispersion strengthening. This study explored the potential of powder metallurgy processing for the fabrication of a high-entropy alloy and other derived compositions with enhanced hardness and strength.