Synthesis and characterisation of Al2O3/Ni-type composites obtained by spark plasma sintering

This paper presents the influence of sintering on the structure, morphology and compressing strength of alumina/nickel composite compacts obtained by spark plasma sintering (SPS). Al₂O₃/Ni composites were prepared by SPS in argon atmosphere at temperatures in the range of 1000–1200 –C with a holding time of 2, 5 and 10?minutes. The heating rate was 200 C?min^?1. These composites have been characterised by X-ray diffraction, SEM and EDX. The relative density and compressive strength of the as-obtained compacts were determined. The results showed that the alumina particles are uniformly dispersed in a quasi-continuous Ni network, and there was no sign of phase changes during sintering. The maximum strength of the alumina/nickel composite with a content of 75 vol. ? Al₂O₃ and 25 vol. ? Ni was about 240?MPa for the samples sintered at 1200?C for 10?minutes.

Special block from the conference RoPM2017 guest edited by Ionel Chicinas, Technical University, Cluj-Napoca.     

Fabrication and characterisation of bulk Al2O3/Mo nanocomposite by mechanical milling and sintering

Abstract

In this study, fabrication and mechanical properties of alumina based ceramic matrix nanocomposite reinforced with 15 and 26·6 vol.-%Mo particles were investigated. Alumina–molybdenum nanocomposite powders were prepared by ball milling of Al and MoO₃ in an SPEX8000 type ball mill. The powder particles were consolidated by cold uniaxial pressing followed by sintering in vacuum atmosphere at 1300 and 1400°C. The structural evaluation of as milled and sintered samples was studied by X-ray diffraction, differential scanning calorimetry and scanning electron microscopy. Sintered samples were examined by hardness measurements and three-point flexural strength. Results show a significant improvement in flexural strength of Al₂O₃–Mo nanocomposites in comparison to monolithic alumina and increases by Mo content. During sintering, grain growth and α-Al₂O₃ to γ-Al₂O₃ transformation occurred. In addition, an increase in temperature of sintering resulted in higher density and hardness of consolidated nanocomposites.     

Production of NiAl–matrix composites by reactive sintering

Abstract

This work was devoted to the development of NiAl–matrix composite and its production by reactive sintering powder metallurgy. Various types of reinforcement (aluminium oxide, silicon and tungsten carbides, titanium silicide) were tested. The best chemical compatibility and the highest hardness and wear resistance were achieved by Al₂O₃ fibres. Electroless nickel plating pretreatment of Al₂O₃ fibres improves both distribution of fibres and hardness of the composite. However, it strongly reduces the wear resistance, probably due to phosphorus content in the nickel coating. In situ formation of NiAl–Al₂O₃ composites by reactive sintering of a pressed powder mixture of Ni, Al and NiO was unsuccessful. Only a small amount of cubic γ-Al₂O₃ was detected after reactive sintering and hence no significant hardness increase was observed.     

Characteristics of Alumina‐Based Inclusions in Low Carbon Al‐Killed Steel under No‐Stirring Condition

Alumina‐based inclusions have a detrimental effect on castability and the surface quality of the LCAK steel sheet, thus they are expected to be removed from the steel. In order to get the detailed transient characteristics of inclusion aggregation and removal after Al addition, laboratory experiments were performed to study the formation of alumina inclusions during Al‐killed process of low carbon steel at 1873 K under no‐stirring condition. The characteristics of the alumina‐based inclusions in terms of amount, size, and morphology were investigated. The results showed that the evolution of the AF (area fraction) and average size of Al₂O₃ inclusions after deoxidation was divided into three stages: 0–9 min, aggregation was dominant; 9–22 min, floating was dominant; after 22 min, both the AF and size decreased slowly. Accordingly, the stirring was suggested to be strengthened in the initial 9 min under stirring condition to promote the removal of large inclusions. Based on the correlation between inclusion morphology and holding time, a simple precipitation and growth mechanism of alumina inclusions was proposed, which consisted of three main stages: precipitation stage of Al₂O₃ single particles, aggregation stage, and sintering stage of aggregated inclusions. And it was implied that the Ostwald‐Ripening can be finished up within 20 min.     

Simultaneous Modification of Alumina and MgO·Al<Subscript>2</Subscript>O<Subscript>3</Subscript> Inclusions by Calcium Treatment During Electroslag Remelting of Stainless Tool Steel

Calcium modification of both alumina and MgO·Al₂O₃ inclusions during protective gas electroslag remelting (P-ESR) of 8Cr17MoV stainless steel and its effect on nitrides and primary carbides were studied by analyzing the transient evolution of oxide and sulfide inclusions in the P-ESR process. The oxide inclusions that were not removed during P-ESR without calcium treatment were found to retain their original state until in as-cast ingot. Calcium treatment modified all MgO·Al₂O₃ and alumina inclusions that had not been removed in the P-ESR process to liquid/partially liquid CaO-Al₂O₃-(MgO) with uniformly distributed elements, in addition to a small proportion of partially modified inclusions of a CaO-MgO-Al₂O₃ core surrounded by a liquid CaO-Al₂O₃. The modification of low-MgO-containing MgO·Al₂O₃ inclusions involves the preferential reduction of MgO from the MgO·Al₂O₃ inclusion by calcium and the reaction of calcium with Al₂O₃ in the inclusion. It is the incomplete/complete reduction of MgO from the spinel by calcium that contributes to the modification of spinels. Alumina inclusions were liquefied by direct reaction with calcium. Calcium treatment during P-ESR refining also provided an effective approach to prevent the formation of nitrides and primary carbides in stainless steel through modifying their preferred nucleation sites (alumina and MgO·Al₂O₃ inclusions) to calcium aluminates, which made no contribution to improving the steel cleanliness.     

Injection moulding of 316L stainless steels reinforced with nanosize alumina particles

Abstract

This study aims to compare the effect of Al₂O₃ nanoparticle additions on the densification and mechanical properties of the injection moulded 316L stainless steels. The 316L stainless steel and Al₂O₃ nanoparticles were dry mixed and moulded using a wax based binder. The critical powder loading for injection moulding were 60 vol.-% for all samples. Debinding process was performed in solvent using thermal method. After the debinding process, the samples were sintered at 1405°C for 60 and 120 min under vacuum. Metallographic examination was conducted to determine the extend of densification and the corresponding microstructural changes. The sintered samples were characterised by measuring tensile strength, hardness and wear behaviour. Wear loss was determined for all the samples after wear testing. All the powders, fracture surfaces of moulded and sintered samples were examined using scanning electron microscope. The sintered density of straight as well as Al₂O₃ nanoparticles reinforced injection moulded 316L stainless steels increases with the increase in sintering time. The additions of Al₂O₃ nanoparticles improve the hardness and wear resistance with the increase of sintering time.     

Interaction of refractory compound nanoparticles with a surfactant in a nickel melt: II. Surface tension and density

The surface tension and density of Ni-S melts with Al₂O₃ or TiN nanoparticles are studied by the sessile drop method using a digital photographic camera and computer processing of images with special-purpose computer programs. The dependences of the surface tension and density of (Ni-S) + (Al₂O₃, TiN) melts on the temperature and the type of introduced refractory compound nanoparticles are determined, and the inversion of the temperature dependence of the surface tension of the Ni-S-Al₂O₃ system is detected. Metallographic analysis of polished sections demonstrates the presence of aluminum, nickel, and sulfur in nonmetallic inclusions at grain boundaries in the first series of experiments and the presence of titanium, nickel, and sulfur in globular nonmetallic inclusions in the second series of experiments.     

Thermodynamic Analysis of Inclusions of Low Melting Point Area in Spring Steel

The activity data of each component of a CaO–SiO₂–Al₂O₃ system were calculated by thermodynamic software Factsage. The composition of low melting point inclusions in a CaO–SiO₂–Al₂O₃–MgO system was analyzed by thermodynamic calculation. The results show that the area of low melting point inclusions first increases then decreases with accumulating the alumina and magnesium oxide contents, respectively; the low melting area of CaO–SiO₂–Al₂O₃–MgO inclusion is the biggest when the content of MgO and Al₂O₃ is 15%. To obtain low melting point inclusions, the alumina and magnesium contents should be approximately controlled to be 15%, and the CaO should be 40%.     

Thermodynamic conditions for inclusions modification in calcium treated steel

The presented paper discussed the fundamental or common thermodynamical relations between calcium-treated aluminium-killed molten steel and non-metallic inclusions. The phase and chemical analyses of inclusions have proven that the correctness of calcium addition can be confirmed and that the analysis of those phenomena can show the effects of previous calcium treatment of aluminium-killed steel. To make the process of manufacturing quality steel successful the factor affecting the necessary calcium addition should be taken into consideration already during the process. Steel, containing too much calcium could have CaS inclusions with a high melting point, while too low contents of calcium cause unsatisfactory modification of solid alumina inclusions to complex liquid calcium-aluminate inclusions. This research included the examination of thermodynamic relations in calcium addition and its reactions with solid Al₂O₃ inclusions. A detailed analysis of the CaO–Al₂O₃ binary system established the modification of solid alumina inclusions via the following intermediate phases: CaO · 6Al₂O₃, CaO · 2Al₂O₃, CaO · Al₂O₃ and liquid phase 12CaO · 7Al₂O₃ and finally again solid CaO, at 1873 K (1600°C). The investigation discusses the further research engaged in consideration of CaO- and Al₂O₃-activities change in each of the quoted intermediate phases. The system as a whole includes details of oxygen activities.     

Improvement of sintering characteristics by selective granulation of high Al2O3 iron ores and ultrafine iron ores

The worldwide steel companies are expected to use low grade iron ores such as pisolitic iron ores, high Al₂O₃ iron ores and ultrafine iron ores etc. in their sinter blends due to the depletion of high grade iron ores or for the economic reason. This study investigated the methods for improving sintering characteristics without deteriorating sintering productivity and sinter quality by blending mini-pellets comprising high Al₂O₃ pisolitic iron ores and ultrafine iron ores containing low alumina. The results showed that the blending of iron ore mini-pellets produced by selective granulation is an effective way to improve sintering productivity and sinter quality without increasing the Al₂O₃ content in sinter as well as to effectively utilise high Al₂O₃ iron ores and ultrafine iron ores in the sintering process.     

Multistage sintering approach to prepare Ni3Al/α-Al2O3 composites

The nickel aluminide intermetallic matrix composites (IMC), Ni₇₆Al₂₄B_0.1 with either 5 or 10 vol pct α-Al₂O₃, were synthesized through a multistage sintering approach from the elemental powders of Ni, Al, and oxide of α-Al₂O₃. An electroless nickel-boron (Ni-B) plating process was adopted to improve the contacted interface between the reinforced oxide ceramics and the metal matrix, as well as to supply the atomic scale boron in the metallic matrix of the IMCs. The entire process comprises steps involving preparing a powdery starting material, sealing it within a metal sheath or can, compacting or cold deforming it, preliminarily heating the compacted material at a relatively low temperature, executing a pore-eliminating (mechanical deforming) process to eliminate the pores resulting from the preceding heating step, and sintering the material at a relatively high temperature to develop a transient liquid phase to heal or to eliminate any microcracks, crazes, or collapsed pores from the previous steps. Most of all, it is important that contact with a heat absorbent material, such as a metal sheath, produces the Ni₂Al₃ phase during preliminary heating. This new phase is a brittle and crispy material with a low melting point (1135 °C). It has been found to play an important role in preventing any significant cracks during the pore-eliminating process and in developing a transient liquid phase in the following 1200 °C sintering step. This multistage sintering with a heat absorbent process is beneficial for producing a product that has large dimensions, a desirable shape, good density, and excellent mechanical properties. The resulting elongation of tensile tests in air reaches 14.6 and 8.9 pct for the present 5 and 10 vol pct powder metallurgy IMCs, respectively.     

Sintering kinetics of YAG ceramics

Solid state reactive （SSR） sintering kinetics was observed for YAG ceramics. There were two densification stages in sin- tering process due to its reaction. After the first stage, samples began to expand, then, the second densification stage began. At a heat- ing rate of 10 ℃/min, the sample warped down and warped back to straight. The apparent activation energy of the first densification process was about 522 kJ/mol for the initial shrinkage of A1203 and Y203 mixed powder green-body, which increased in the follow- ing process due to the solid state reaction. In the second densification stage, synthesis reaction of YAG still worked. Green-bodies processed with higher heating rate got more shrinkage at the same temperature than lower heating rate green bodies. And its kinetic field diagram was abnormal, compared with that of other reported ceramics, such as Al203. It was found that the reaction of YAG provided positive effect to the sintering driving force. The apparent activation energy for densification of SSR YAG sintered in ArH5 atmosphere was 855 kJ/mol at temperature holding sintering. And the apparent activation energy for grain growth was 1053 kJ/mol.     

Effect of heat treatment on compressive properties of open cell Al/Al2O3 composite foams

Abstract

The sintering and dissolution process was used to produce open cell Al/Al₂O₃ composite foams with a relative density of 0·25–0·40 and a pore size of 112–400 μm. The compressive properties of as fabricated and T6 heat treated Al/Al₂O₃ composite foams were investigated. After T6 heat treatment, the yield strength of the open cell Al/Al₂O₃ composite foams is increased relative to the untreated material. T6 heat treatment gives rise to a mean 36% increase in the compression yield strength of the open cell Al/Al₂O₃ composite foams. The yield strength of as fabricated and T6 heat treated Al/Al₂O₃ composite foams shows a significant dependence on the relative density and also exhibits a distinct dependence on the pore size. After T6 heat treatment, the influence of the relative density and pore size on the compressive behaviour of Al/Al₂O₃ composite foams becomes more distinct.     

Enhanced densification of cavitated dispersion-strengthened aluminum by thermal cycling

We report experimental data of creep cavity shrinkage for dispersion-strengthened-cast aluminum with about 23 vol pct submicron Al₂O₃ dispersoids, annealed isothermally or subjected to thermal cycling without applied stress. Thermal cycling is found to increase the rate of densification by a factor of 3 to 5.5 relative to isothermal annealing at the upper cycling temperature, allowing for recovery of full theoretical density in a shorter time. Isothermal densification is discussed in light of a diffusive cavity shrinkage mechanism, and a model considering thermal mismatch stresses is employed to rationalize the enhanced rate of densification observed during thermal cycling. Intermittent thermal-cycling densification is shown to improve creep life of dispersion-strengthened aluminum through the suppression of tertiary damage accumulation processes.     

Control of Non‐metallic Inclusions by Slag‐metal Reactions for High Strength Alloying Steels

A laboratory study was carried out to investigate non‐metallic inclusions in high strength alloying steel refined by high basicity slag. The results indicated that the inclusions were mainly of the CaO? MgO? Al₂O₃ system, Al₂O₃? MgO and MgO‐based inclusions. The steel/slag reaction time and Al₂O₃ content in slag had a great effect on inclusions characteristics. With the reaction time increasing from 30 to 180 minutes, inclusions experienced a transformation process: from mainly Al₂O₃? MgO system and MgO‐based inclusions to spherical CaO? MgO? Al₂O₃ system inclusions surrounded by a lower melting temperature surface layer of CaO? Al₂O₃. Formation and transformation mechanisms of the inclusions were given based on the results. It was also found that with Al₂O₃ content in slag reduced from 40% to 30%, [Mg] contents in steel melts were increased and MgO in slag reached saturation, which contributed to the formation of more MgO‐based inclusions and a more scattered inclusion composition distribution after 90 min reaction.     

Effects of powder processing on densification of titanium diboride based cermets

Abstract

The sinterability of TiB₂-Ni₃(Al,Ti) based cermets has been significantly improved by aggressive milling of the starting TiB₂-Ni-TiAl₃ powder mixtures. This technique improves not only liquid spreading by reducing TiAl₃ particle size but also eliminates alumina agglomerates and the associated porosity found after vacuum sintering. Liquid phase sintering of TiB₂-Ni-TiAl₃ powder mixtures involves the presence of Ni based secondary borides at low temperatures (1200°C), which react afterwards with TiAl₃ particles leading to the formation of the final TiB₂-Ni₃(Al,Ti) eutectic liquid. Apart from improving liquid spreading around TiB₂ grains, aggressive milling is also found to disperse alumina agglomerates, which reduces the porosity associated to these particles. By this refined procedure, the amount of binder phase required for full densification of TiB₂ cermets by sinter hipping has been reduced from a previous limit of 16 vol.-% to 10 vol.-%. The hardness of these TiB₂-10 vol.-%Ni₃(Al,Ti) cermets is in the range of ultrafine WC-Co hardmetals in spite of their much coarser microstructure.     

Application of PAP-2 aluminum powder to produce powdered composite materials: The features of technology,structure, and physicomechanical properties of composites. Part I. Process approaches providing the formation of composite materials and applied procedures for determining their physicomechanical properties

Composites Al/Al₂O₃ (lamellar cermet matrix)–filler (discrete metallic fibers, duralumin chips, graphite particles, fused corundum grains, and technical alumina spherulites) are fabricated. To form the lamellar cermet matrix, industrially produced PAP-2 aluminum powder was used. This powder consists of scaled particles with stearin coating (the specific surface of the powder is 4.1322 m²/g, and its particle size varies from 0.03 to 10 μm). In order to form the composites, the following main process operations were used: heat treatment of the PAP-2 powder in air to burn out stearin from the particle surface and replace it with a passivating alumina film, mixing of the thus formed powder product with a filler, and compaction and reaction sintering of powder billets in the filtration burning mode in air. To fabricate the Al/Al₂O₃–C composite, a new approach based on the saponification chemical reaction of stearin is proposed. This reaction runs between stearin on the surface of aluminum particles and caustic soda, which is the product of hydrolysis of the diluted liquid glass introduced into initial powder. The reaction products (sodium stearate and glycerol) are decomposed during the subsequent heat treatment in air with the formation of a coke residue on the particle surface. The physicochemical properties of the composites were determined using standard and conventional procedures.     

On the interaction between alumina batch and cryolite-alumina melt

The influence produced by the bulk density of alumina powder on the rate of its dissolution in a cryolite-alumina melt of the composition, wt %, 5.5 CaF₂, 1.5 MgF₂, 0.3 Al₂O₃, 2.28 CR is studied. The melt temperature is 950°C; the dissolution rate is determined visually and by changes in the concentration of aluminum oxide in the melt. It is discovered that the dissolution rate of alumina increases in proportion to its bulk density.     

Sintering a disperse mixture of W-Sc2O3 powders

The effect of additions of scandium oxide (1, 5, and 10 vol. %) on compaction during sintering of a disperse mixture of W-Sc₂O₃ powder at 2000°C has been studied. It has been found that the scandium oxide particles activate compaction during heating and conversely retard shrinkage of tungsten in the stage of isothermal soaking. The kinetics of compaction during sintering is determined by the geometry of the heterophase system. Depending on how much the tungsten and scandium oxide particles increase in size, the nature of thestructure changes markedly from matrix-statistical to statistical.