alpha-SiAlON-SiC composites obtained by gas-pressure sintering and hot-pressing

The objective of this work was the obtaining in situ of alpha-SiAlON-SiC composite, using an alternative rare-earth oxide mixture, RE2O3, as sintering additive, by two different sintering processes. As sintering additive, 20 vol.% of AlN-RE2O3 in a molar ratio of 90: 10 was mixed to the alpha-Si3N4 powder. In the Si3N4-AlN-RE2O3 powder mixture, 0, 10, 15 and 20wt.% of SiC were added. The powder batches were milled, dried and compacted by cold isostatic pressing. Two different sintering processes were used: gas-pressure sintering at 1950 degrees C for 1 h under 1.5 MPa of N-2 atmosphere, or uniaxial hot-pressing at 1750 degrees C, for 30 min under pressure of 20 MPa. The sintered samples were characterized by X-ray diffraction, scanning electron microscopy and mechanical properties. XRD patterns indicate only alpha-SiAlON (alpha') and beta-SiC as crystalline phases. It was observed that the SiC addition did not influence the alpha-SiAlON formation, although the growth of elongated alpha'-grains is substantially decreased. The hot-pressed composites presented better mechanical properties, exhibiting fracture toughness of 5 MPa m(1/2) and hardness around 21.5 GPa. (c) 2007 Elsevier B.V. All rights reserved.

Development of alpha-SiAlON-SiC ceramic composites by liquid phase sintering

In this work, in situ alpha-SiAlON-SiC ceramic composites were obtained,by, liquid phase sintering, using SiC as reinforcement. Different beta-SiC powder contents (0-20 wt.%), were added to Si3N4-AlN-RE2O3. powder mixtures, and compacted by cold isostatic pressing. The samples were sintered at 1950 degrees C for 1 h, in N-2 atmosphere. Sintered: samples were characterized by relative density, weight loss, X-ray diffraction and scanning electron microscopy. Furthermore, mechanical properties such as hardness and fracture toughness were determined by Vickers indentation method. Lattice parameters of the alpha' phase did not considerably change with increase of SiC content. However, morphology, average grain size and aspect ratio of the alpha' phase were considerably changed with increase of the SiC content. These behavior influences significantly the mechanical properties of this hard ceramic composite. (C) 2006 Elsevier Ltd. All rights reserved.

Obtenção in situ do compósito alfa-SiAlON-SiC

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Phase and microstructural evolution during the heat treatment of Sm-Ca-alpha-sialon ceramics

The phase and microstructural evolution of multi-cation Sm-Ca-alpha-sialon ceramics was investigated. Six samples were prepared, ranging from a pure Sm-sialon to a pure Ca-sialon, with calcium replacing samarium in 20 eq% increments, thus maintaining an equivalent design composition in all samples. After pressureless sintering at 1820 degreesC for 2 It, all samples were subsequently heat treated up to 192 h at 1450 and 1300 degreesC. The amount of grain boundary glass in the samples after sintering was observed to decrease with increasing calcium levels. A M-ss' or M-ss',-gehlenite solid solution was observed to form during the 1450 degreesC heat treatment of all Sm-containing samples, and this phase forms in clusters in the high-Sm samples. The thermal stability of the alpha-sialon phase was improved in the multi-cation systems. Heat treatment at 1300 degreesC produces SmAlO3 in the high-Sm samples, a M-ss',-gehlenite solid solution in the high-Ca samples, and a Sm-Ca-apatite phase in some intermediate samples. (C) 2002 Elsevier Science Ltd. All rights reserved.

Thermal stability of mixed-cation alpha-sialon ceramics

A series of alpha-sialon (alpha') compositions containing mixed stabilising cations were prepared, by introducing additional CaO to a basic Sm alpha-sialon compositions. The thermal stability of these Sm-Ca-containing alpha-sialon phases was investigated using XRD, SEM and EDXS techniques. It was found that the addition of calcium into the Sm alpha-sialon systems greatly improved the stability of the alpha-sialon phases. Calcium was found to be incorporated into the alpha-sialon structure, coexistent with the samarium, and partitioning of the calcium and samarium was observed between the alpha' phase and grain boundary phases. This indicates a technique which may be used to improve the thermal stability of the alpha' phase while maintaining good refractory phases at the gialon grain boundaries. (C) 2003 Elsevier Science B.V. All rights reserved.

alpha-SiAlON ceramics with elongated grain morphology using an alternative sintering additive

In this work, the use of a natural yttrium oxide and rare earth oxide solid solution (CRE2O3) as stabilizers of the alpha-Si3N4 phase to form alpha-SiAlON has been investigated. This oxide mix is produced at FAENQUIL-DEMAR, at a cost of only 20% of pure commercial Y2O3. Two alpha-SiAlONs using pure Y2O3 or CRE2O3 have been prepared, using mixes of 20% by volume of a molar fraction of 9:1 of AlN to Y2O3 or AlN to CRE2O3, respectively, with 80% alpha-Si3N4. Samples were gas pressure-sintered at 1900 degreesC, under 1.5 MPa of N-2 for 60 min. Both compositions yielded alpha-SiAlON ceramics with high relative densities (98% t.d.), hardness of 18 GPa and fracture toughness of 5 Mpa m(1/2), with homogeneous microstructures composed of elongated alpha-SiAlON grains with aspect ratios of 5. It is concluded that the mixed rare earth concentrate (CRE2O3) can be used to produce alpha-SiAlON ceramics with similar microstructures and mechanical properties of alpha-SiAlON ceramics fabricated using pure Y2O3, but with the advantage of its lower production cost. (C) 2004 Elsevier B.V All rights reserved.

Microstructural evidence for the mechanism of the alpha-beta phase transformation in ytterbium SiAlON ceramics

Detailed microstructural evidence for the mechanism of the alpha-beta phase transformation in ytterbium SiAlON ceramics is presented. Grains, which show partial transformation, have been examined using transmission electron microscopy. We suggest that the transformation proceeds as a discernable reaction front and the accompanying lattice mismatch is accommodated be a series of complex dislocations. The stabilizing cation is ejected from the transformed alpha- phase and diffuse along the dislocation to accumulate as isolated pockets in a way similar to that observed in metal systems and termed pipe diffusion. High-resolution electron microscopy reveals the details of each of these features.

Effects of Fe addition on the mechanical and thermo-mechanical properties of SiC/FeSi2/Si composites produced via reactive infiltration

Remaining silicon in SiC-based materials produced via reactive infiltration limits their use in high-temperature applications due to the poor mechanical properties of silicon: low fracture toughness, extreme fragility and creep phenomena above 1000 °C. In this paper SiC–FeSi2 composites are fabricated by reactive infiltration of Si–Fe alloys into porous Cf/C preforms. The resulting materials are SiC/FeSi2 composites, in which remaining silicon is reduced by formation of FeSi2. For the richest Fe alloys (35 wt% Fe) a nominal residual silicon content below 1% has been observed. However this, the relatively poor mechanical properties (bending strength) measured for those resulting materials can be explained by the thermal mismatch of FeSi2 and SiC, which weakens the interface and does even generate new porosity, associated with a debonding phenomenon between the two phases.

α′ phase stability in Nd-Li-sialon systems

The formability and stability of the alpha-sialon (alpha') phase was investigated in multi-cation Nd-Li-sialon systems. Four samples were prepared, ranging from a pure Nd-sialon to a pure Li-sialon, with two intermediate samples being prepared with either lithium or neodymium replacing the other alpha'-stabilising additive by 20 eq.%, as to maintain an equivalent design composition in all samples. After sintering, all samples were subsequently heat treated up to 192 h at 1450 and 1300 degreesC. While significant quantities of the beta'-sialon (beta' phase were found in most samples, the high-lithium Li-Nd-sialon sample was found to be almost pure a' phase after sintering. Furthermore, the long-term stability of the a' phase on heat treatment was also found to be superior in both multi-cation samples than in either of the single-alpha'-stabilising-cation samples. This is thought to be related to improved retention of the lithium in the multi-cation systems, as much of the lithium was found to volatilise during sintering in the neodymium-free sample. (C) 2002 Elsevier Science Ltd. All rights reserved.

Role of reinforcement/matrix interfacial strength in fatigue crack propagation in particulate SiC reinforced aluminum alloy 8090

A study has been made of the influence of the reinforcement/matrix interfacial strength on fatigue crack propagation in a powder metallurgy aluminum alloy 8090-SiC particulate composite. The interfacial region has been altered by two separate routes, the first involving aging of the 8090 matrix, with the subsequent formation of precipitate free zones at the boundaries, and the second consisting of oxidizing the surface of the SiC particles before their incorporation into the composite. In the naturally aged condition, oxidation of the SiC leads to a reduction in fatigue crack growth resistance at higher values of stress intensity range ΔK. This is due to a proportion of the crack growth occurring through voids formed in association with many of the weak SiC interfaces which have retained a layer of thick surface oxide after processing. On overaging no difference in crack growth rate is discernible between the oxidized and unoxidized SiC composites. It is proposed that this is due to similar levels of interfacial weakening having occurred in both composites, indicating that this is an important factor in the reduction of the high ΔK crack growth resistance of the unoxidized SiC composite on aging.

Influence of the substitution of Y2O3 for CeO2 on the mechanical and microstructural properties of silicon nitride

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Fiber-reinforced ceramics for thermostructural applications, produced by polymer impregnation pyrolysis

Several CFCC (Continuous Fiber Composite Ceramics) production processes were tested, concluding that PIP (Polymer Impregnation, or Infiltration, Pyrolysis) and CBC (Chemically Bonded Ceramics) based procedures have interesting potential applications in the construction and transportation fields, thanks to low costs to get potentially useful thermomechanical performances. Among the different processes considered during the Doctorate (from the synthesis of new preceramic polymers, to the PIP production of SiC / SiC composites) the more promising results came from the PIP process with poly-siloxanes on basalt fabrics preforms. Low processing time and costs, together with fairly good thermomechanical properties were demonstrated, even after only one or two PIP steps in nitrogen flow. In alternative, pyrolysis in vacuum was also tested, a procedure still not discussed in literature, but which could originate an interesting reduction of production costs, with only a moderate detrimental effect on the mechanical properties. The resulting CFCC is a basalt / SiCO composite that can be applied for continuous operation up to 600°C, also in oxidant environment, as TG and XRD demonstrated. The failure upon loading is generally pseudo-plastic, being interlaminar delamination the most probable rupture mechanism. . The strength depends on several different factors (microstructure, polymer curing and subsequent ceramic phase evolution, fiber pull-out, fiber strength, fiber percentage) and can only be optimized empirically. In order to be open minded in selecting the best technology, also CBC (Chemically Bonded Ceramics) matrixes were considered during this Doctorate, making some preliminary investigations on fire-resistant phosphate cements. Our results on a commercial product evidenced some interesting thermomechanical capabilities, even after thermal treatments. However the experiments showed also phase change and possible cracking and deformations even on slow drying (at 130°C) and easy rehydration upon exposure to environmental humidity.

High-Performance-Tensile-Strength Alpha-Grass Reinforced Starch-Based Fully Biodegradable Composites

Though there has been a great deal of work concerning the development of natural fibers in reinforced starch-based composites, there is still more to be done. In general, cellulose fibers have lower strength than glass fibers; however, their specific strength is not far from that of fiberglass. In this work, alpha-fibers were obtained from alpha-grass through a mild cooking process. The fibers were used to reinforce a starch-based biopolymer. Composites including 5 to 35% (w/w) alpha-grass fibers in their formulation were prepared, tested, and subsequently compared with those of wood- and fiberglass-reinforced polypropylene (PP). The term “high-performance” refers to the tensile strength of the studied composites and is mainly due to a good interphase, a good dispersion of the fibers inside the matrix, and a good aspect ratio. The tensile strength of the composites showed a linear evolution for fiber contents up to 35% (w/w). The strain at break of the composites decreased with the fiber content and showed the stiffening effects of the reinforcement. The prepared composites showed high mechanical properties, even approaching those of glass fiber reinforced composites

Anodization mechanism on SiC nanoparticle reinforced al matrix composites produced by power metallurgy

Specimens of aluminum-based composites reinforced by silicon carbide nanoparticles (Al/SiCnp) produced by powder metallurgy (PM) were anodized under voltage control in tartaric-sulfuric acid (TSA). In this work, the influence of the amount of SiCnp on the film growth during anodizing was investigated. The current density versus time response and the morphology of the porous alumina film formed at the composite surface are compared to those concerning a commercial aluminum alloy (AA1050) anodized under the same conditions. The processing method of the aluminum alloys influences the efficiency of the anodizing process, leading to a lower thicknesses for the unreinforced Al-PM alloy regarding the AA1050. The current density versus time response is strongly dependent on the amount of SiCnp. The current peaks and the steady-state current density recorded at each voltage step increases with the SiCnp volume fraction due to the oxidation of the SiCnp. The formation mechanism of the anodic film on Al/SiCnp composites is different from that occurring in AA1050, partly due the heterogeneous distribution of the reinforcement particles in the metallic matrix, but also to the entrapment of SiCnp in the anodic film.

Fracture toughness of SIC, Si3N4, and sialon ceramics using controlled surface flaws

Knoop and Vickers indentation cracks have frequently been used as model 'precracks' in ceramic bend specimens for fracture toughness (K1c) determination. Indentation residual stress reduces the measured K1c but can be removed or accounted for by grinding, annealing, or modelling. Values of K1c are obtained for four materials using Vickers indentations and an improved stress intensity factor. Methods for residual stress removal or incorporation are compared, and the most reliable stress removal alternative is identified for each material. © 1996 The Institute of Materials.