In-situ synthesis of a ZrB2–based composite powder using a mechanochemical reaction for the zircon/magnesium/boron oxide/graphite system

A ZrSiO4/B2O3/Mg/C system was used to synthesize a ZrB2-based composite through a high-energy ball milling process. As a result of the milling process, a mechanically induced self-sustaining reaction (MSR) was achieved in this system. A composite powder of ZrB2–SiC–ZrC was prepared in situ by a magnesiothermic reduction with an ignition time of approximately 6 min. The mechanism for the formation of the product was investigated by studying the relevant subreactions, the stoichiometric amount of B2O3, and thermal analysis.Peer reviewe

High temperature oxidation resistance of (Ti,Ta)(C,N)-based cermets

Cermets based on titanium–tantalum carbonitride were oxidized in static air between 800 °C and 1100 °C for 48 h. The thermogravimetric and microstructural study showed an outstanding reduction in the oxidation of more than 90% when the Ta content was increased. In cermets with low Ta content, the formation of a thin CoO/Co3O4 outer layer tends to disappear by reacting with the underlying rutile phase, which emerges at the surface. However, in cermets with higher Ta content, the formation of an external titanate layer, observed even at a low temperature, appears to prevent the oxygen diffusion and the oxidation progressionPeer reviewe

Kinetics of high-temperature oxidation of (Ti,Ta)(CN)-based cermets

The kinetics of the high-temperature oxidation of titanium–tantalum carbonitride-based cermets with different Ti/Ta ratios was studied. Isothermal oxidation tests were conducted under static air for 48 h at temperatures between 700 °C and 1200 °C. The oxidation satisfied the parabolic kinetics, characteristic of the existence of a protective oxide layer. The apparent activation energy suggests the rate-controlling process during oxidation is the simultaneous inward and outward diffusion of oxygen and titanium, respectively, through the formed protective layer, consisting mainly of a rutile phase. A higher Ta(V) content in the rutile decreased the oxygen diffusivity due to the reduction of oxygen vacancy concentration.Peer reviewe

Room temperature mechanosynthesis of the La 1-xSr xMnO 3±δ (0≤x≤1) system and microstructural study

Monophase nanocrystalline powders belonging to the La 1-xSr xMnO 3±δ system (0≤x≤1) with a perovskite structure have been obtained by mechanochemistry synthesis using a planetary ball milling equipment from La 2O 3, SrO, and Mn 2O 3 mixtures. The solid state reaction was complete after one hour of milling treatment. For all the compositional range, the diffraction domain was very small and the structure appeared as a pseudo cubic perovskite. After annealing at 1100 °C under static air, the symmetry evolution due to the La substitution by Sr was analyzed by X-ray and electron diffraction. Samples with x=0, 0.25, 0.5, and 0.75 were assigned to R-3c space group (1 6 7) in the rhombohedral system and perovskite structure. However, the symmetry of the last term of the system (x=1), SrMnO 3±δ sample, changed to P6 3/mmc space group (1 9 4) in the hexagonal system. The terms with x=0.8, 0.85, and 0.9 presented mainly rhombohedral symmetry. © 2012 Elsevier Inc.Peer Reviewe

Formation mechanism of ZrB2-Al2O3 nanocomposite powder by mechanically induced self-sustaining reaction

ZrB2-Al2O3 nanocomposite powder was produced by aluminothermic reduction in Al/ZrO2/B2O 3 system. In this research, high energy ball milling was used to produce the necessary conditions to induce a mechanically induced self-sustaining reaction. The ignition time of the composite formation was found to be about 13 min. The synthesis mechanism in this system was investigated by examining the corresponding sub-reactions as well as changing the stoichiometry of reactants. Thermal behavior of the system was also studied. © 2013 Springer Science+Business Media New York.Peer Reviewe

Inverse core-rim microstructure in (Ti,Ta)(C,N)-based cermets developed by a mechanically induced self-sustaining reaction

Cermets with a nominal composition (Ti 0.8Ta 0.2C 0.5N 0.5- 20 wt.% Co) were synthesised by a mechanically induced self-sustaining reaction (MSR) process from stoichiometric elemental powder blends. The MSR allowed the production of a complex (Ti,Ta)(C,N) solid solution, which was the raw material used for the sintering process. The pressureless sintering process was performed at temperatures between 1400 °C and 1600 °C in an inert atmosphere. The microstructural characterisation showed a complex microstructure composed of a ceramic phase with an unusual inverse core-rim structure and a Ti-Ta-Co intermetallic phase that acted as the binder. © 2011 Elsevier Ltd. All rights reserved.Peer Reviewe

Influence of the Test Configuration and Temperature on the Mechanical Behaviour of WC-Co

In this work, the effect of the test configuration and temperature on the mechanical behaviour of cemented carbides (WC-Co) with different carbide grain sizes (dWC) and cobalt volume fractions (VCo), implying different binder mean free paths ( Co), was studied. The mechanical strength was measured at 600º C with bar-shaped specimens subjected to uniaxial four-point bending (4PB) tests and with disc specimens subjected to biaxial ball-on-three-balls (B3B) tests. The results were analysed within the frame of theWeibull theory and compared with strength measurements performed at room temperature under the same loading conditions. A mechanical degradation greater than 30% was observed when the samples were tested at 600ºC due to oxidation phenomena, but higherWeibull moduli were obtained as a result of narrower defect size distributions. A fractographic analysis was conducted with broken specimens from each test configuration. The number of fragments (Nf) and the macroscopic fracture surface were related to the flexural strength and fracture toughness of WC-Co. For a given number of fragments, higher mechanical strength values were always obtained for WC-Co grades with higher KIc. The observed differences were discussed based on a linear elastic fracture mechanics (LEFM) model, taking into account the effect of the temperature and microstructure of the cemented carbides on the mechanical strength.Junta de Andalucía P12-TEP-262

Toughening of complete solid solution cermets by graphite addition

(Ti0.95Ta0.05)(C0.5N0.5)-Co complete solid solution cermets (CSCs) were developed by a mechanochemical synthesis process and a pressureless sintering method. The effect of different percentages of graphite used as a sintering additive on the nature of the binder phase and the mechanical properties of the cermets was investigated. Microstructural and mechanical characterisations were carried out by X-ray diffraction, optical microscopy, scanning electron microscopy, transmission electron microscopy, energy-dispersive X-ray spectroscopy, Vickers hardness, indentation fracture toughness and nanoindentation. The addition of graphite modified the carbon activity during sintering, reducing the dissolution of carbonitride ceramic particles into the molten binder. The amount of Ti and Ta remaining in the binder after sintering gradually decreased as the amount of graphite added increased, which induced a change in the nature of the binder phase. When no graphite was added, the binder consisted of the brittle TixTa1-xCo2 intermetallic phase. With the increase in the amount of graphite added, the formation of more ductile phases, such as TixTa1-xCo3 and α-Co, was observed, causing a significant improvement in the toughness of the cermets.Peer reviewe

Sintering by SPS of ultrafine TiCx N1-x powders obtained using mechanically induced self sustaining reaction

[EN] In this work high purity and nanometer character titanium carbonitride TiCx N1-x powders were obtained by mechanically induced self sustaining reaction (MSR) in a high-energy planetary ball mill, from a mixture of titanium with graphite or carbon nanofiber (CNFs) in a nitrogen atmosphere. A promising method for developing these materials is the coupling of the MSR with SPS sintering technique. The product is sintered at 1400 ºC and 1700 ºC, obtaining a completely dense monolithic ceramic (>99% t.d). In this work, the influence of SPS treatment and carbon precursor on material microstructures was studied and the main mechanical properties of the end material were evaluated[ES] En el presente trabajo se han obtenido carbonitruros de titanio TiCx N1-x de alta pureza y con carácter nanométrico, por molienda reactiva (MSR) de alta energía en un molino planetario, a partir de la mezcla de titanio con grafito o nanofibras de carbono (CNFs) en una atmósfera de nitrógeno. Una metodología prometedora para el desarrollo de estos materiales consiste en el acoplamiento de la técnica MSR con el sinterizado por SPS. El producto obtenido se ha sinterizado a 1400 ºC y 1700 ºC, obteniéndose una cerámica monolítica totalmente densa (>99% d.t). En este trabajo se analizan las distintas microestructuras obtenidas en función del precursor de carbono y el tratamiento de SPS, evaluando las principales propiedades mecánicas de los materiales resultantes.Este trabajo ha sido llevado acabo con financiación procedente de los proyectos del plan nacional MAT2006-01783 y MAT2006-04911.Borrell Tomás, MA.; Fernández, A.; Torrecillas, R.; Córdoba, J.; Avilés, M.; Gotor, F. (2010). Sinterización por SPS de polvos ultrafinos de TiCxN1-x obtenidos mediante reacciones de autopropagación inducidas mecánicamente. Boletín de la Sociedad Española de Cerámica y Vidrio. 49(5):357-360. http://hdl.handle.net/10251/64404S35736049