Amino Acids Aided Sintering for the Formation of Highly Porous FeAl Intermetallic Alloys.
ABSTRACT: 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 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:The article presents an investigation on the effectiveness of nanostructured titanium-10 wt% 45S5 Bioglass-1 wt% Ag composite foams as a novel class of antibacterial materials for medical applications. The Ti-based composite foams were prepared by the combination of mechanical alloying and a "space-holder" sintering process. In the first step, the Ti-10 wt% 45S5 Bioglass-1 wt% Ag powder synthesized by mechanical alloying and annealing mixed with 1.0 mm diameter of saccharose crystals was finally compacted in the form of pellets. In the next step, the saccharose crystals were dissolved in water, leaving open spaces surrounded by metallic-bioceramic scaffold. The sintering of the scaffold leads to foam formation. It was found that 1:1 Ti-10 wt% 45S5 Bioglass-1 wt% Ag/sugar ratio leads to porosities of about 70% with pore diameter of about 0.3-1.1 mm. The microstructure, corrosion resistance in Ringer's solution of the produced foams were investigated. The value of the compression strength for the Ti-10 wt% 45S5 Bioglass-1 wt% Ag foam with 70% porosity was 1.5 MPa and the Young's modulus was 34 MPa. Silver modified Ti-10 wt% 45S5 Bioglass composites possess excellent antibacterial activities against Staphylococcus aureus. Porous Ti-10 wt% 45S5 Bioglass-1 wt% foam could be a possible candidate for medical implants applications.
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: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:Sintering is a key technology for processing ceramic and metallic powders into solid objects of complex geometry, particularly in the burgeoning field of energy storage materials. The modeling of sintering processes, however, has not kept pace with applications. Conventional models, which assume ideal arrangements of constituent powders while ignoring their underlying crystallinity, achieve at best a qualitative description of the rearrangement, densification, and coarsening of powder compacts during thermal processing. Treating a semisolid Al-Cu alloy as a model system for late-stage sintering-during which densification plays a subordinate role to coarsening-we have used 3D X-ray diffraction microscopy to track the changes in sample microstructure induced by annealing. The results establish the occurrence of significant particle rotations, driven in part by the dependence of boundary energy on crystallographic misorientation. Evidently, a comprehensive model for sintering must incorporate crystallographic parameters into the thermodynamic driving forces governing microstructural evolution.
Project description: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:The stoichiometry of titanium carbide (TiCx) particles is important in determining particle properties. Spherical TiCx powders with particle sizes of 1-5 ?m were produced by self-propagating high-temperature synthesis (SHS) in 30 wt.% Al-, 30 wt.% Cu-, and 30 wt.% Fe-Ti-C systems, respectively. To measure the compositions of the carbide powders, atom probe tomography (APT) tip specimens were carefully prepared by using a focus ion-beam milling method. APT analysis revealed that the TiCx particles formed in Al-, Cu-, and Fe-Ti-C systems are highly substoichiometric. The results are consistent with observations of the TiCx particles with a high content of oxygen and a certain amount of secondary metallic elements (Al, Cu, and Fe).
Project description:In this work, Ni particles/PA12 powders (Ni/PA12) and graphite oxide (GO)-encapsulated Ni particles/PA12 powders (GO-Ni/PA12) composite powders were prepared by defect-included electroless plating technique, and its laser sintered behaviour was investigated. Results showed that a lot of defects could formed on the surface of CH3COOH etched PA12 powders. The defects would induce Ni and GO-Ni particles independently plated on the PA12 surface. Adding GO in the plating solution would facilitate the deposition of Ni particles, GO, and NiO on the PA 12 surface, but inhibit the growth and the crystallinity of the Ni particles. The SLS process involved the contact of PA12 powders, the formation of sintering neck, the growth of sintering neck and the formation of fused solid. Sintering process could facilitate the re-arrangement of Ni particles due to surface tension and the growth of sintering neck. The Ni particles had well wettability, and the interfaces between Ni particles and PA 12 were contacted soundly. The tensile strength and bending strength of the 10 W-sintered Ni/PA12 specimen were 50?MPa and 60?MPa. But SLS process caused the serious aggregation of GO-Ni particles due to higher concentration, activity and surface area of GO-Ni particles.
Project description:In this study, a novel self-assembling hydrogen generation powder comprised of 80Al-10Bi-10Sn wt.% was prepared using the gas atomization method and then collected in an air environment. The morphological and hydrolysis properties of the powders were investigated. The results indicated that the powders formed unique core/shell microstructures with cracked surfaces and (Bi, Sn)-rich phases distributed on the Al grain boundaries. The powders exhibited good oxidation resistance and reacted violently with distilled water at temperatures as low as 0 °C. Furthermore, at 30 °C, the powders exhibited a hydrogen conversion yield of 91.30% within 16 minutes. The hydrogen produced by this powder could be directly used in proton exchange membrane fuel cells. The mechanisms of the hydrolysis reactions were also analyzed.
Project description:Halogen-free flame-retardant polystyrene (PS) foams prepared by supercritical carbon dioxide (SC-CO2) foaming have been achieved. The flame-retardants include expandable graphite (EG) and melamine phosphate (MP), and their influence on the foamability, decomposition behavior, fire performance, and mechanical properties of PS foams were investigated. It has been shown that flame retardants can generate inert gases and catalyze the char formation from PS, and the formed thick char layer with a notable barrier property can greatly decrease the heat release of PS foams. The addition of triphenyl phosphate (TPP) or hexaphenoxycyclotriphosphazene (HPCTP), which acts as a flame-retardant plasticizer, can obviously improve the foamability and fire performance of the foams. TPP or HPCTP can generate active phosphorous species and phenoxyl radicals to enhance the gas phase flame-retardant effect; therefore, the flame-retarded PS foams (with 25 wt % MP/EG) achieve HF1 and V-0 ratings, with limiting oxygen index (LOI) values of 30.1 or 29.6%, respectively. The numerical assessment of synergistic effects of TPP and HPCTP on further enhancing flame retardancy of PS foams has been provided by the microcalorimeter (MCC) test. Further X-ray photoelectron spectroscopy (XPS) investigation on char residues of PS foams demonstrates the formation of the P-O-C and other stable structures.