Preliminary studies in the processing and characterization of Al2O3/SnO2 laminated composites

All oxide composites (reinforcement and matrix both being oxides) exhibit high temperature oxidation resistance in addition to high strength and hardness. A major drawback of these materials is that the oxide fiber and oxide matrix tend to react, which strengthens the interface and therefore drastically reduces the damage tolerance. To overcome this problem, a mechanically weak interphase material, which also serves as a diffusion barrier, is generally used. One such materials system is tin dioxide (SnO₂) in alumina-based composites. Previous attempts to fabricate such alumina matrix composites have been unsuccessful due to the higher temperatures needed to densify Al₂O₃ coupled with the fact that SnO₂ decomposes to SnO in reducing environments. SnO has a relatively low melting point (1125 °C). In this paper we report the successful fabrication of Al₂O₃/SnO₂, laminated composites and some observations on microstructural and mechanical characterization of the laminates. As expected from the phase diagram, no chemical compound formation was observed between Al₂O₃ and SnO₂ which means that no primary chemical bonding developed between individual laminae. TEM observations showed, however, a strong mechanical interlocking at the SnO₂/Al₂O₃ interfaces. In spite of the relatively strong interfacial bond, cracks did deflect. Our microstructural studies showed that SnO₂ served as a weak interphase material.     

Coefficients of thermal expansion of some laminated ceramic composites

The coefficients of thermal expansion (CTE) were determined for several non-fibrous alumina-based laminated ceramic composites. The results were compared with the CTE values predicted by the modified equations of Schapery and Chamis. Both models are identical in the longitudinal direction and showed differences from experimental CTE of 2.3 and 4.1% for alumina/barium zirconate (Al₂O₃/BaZrO₃) and alumina/tin dioxide (Al₂O₃/SnO₂) composites, respectively. For Al₂O₃/BaZrO₃ in the transverse direction, Schapery's model showed a 1.9% difference while Chamis’ model showed a 7.5% difference. For the Al₂O₃/SnO₂ in the transverse direction, Schapery's model had an 8.2% difference while Chamis’ model showed only a 2.3% difference. Results for alumina/calcium titanate (Al₂O₃/CaTiO₃) laminates showed larger differences, 27.6% in longitudinal CTE and differences of 9.6 and 19.8% transverse CTE for the Schapery and Chamis models, respectively. These differences were attributed to the formation of cracks that occurred in this composite system during processing because of the large CTE mismatch between Al₂O₃ and CaTiO₃. Results for Al₂O₃/BaZrO₃ and Al₂O₃/SnO₂ composites showed that for continuous laminae both the Schapery and Chamis models were adequate predictors of CTE for the systems.     

Glass-ceramic bonding in alumina/CBN abrasive systems

A glass-ceramic bond which can be applied in alumina/CBN abrasive systems was developed by the method of liquid-phase sintering of a homogenized mixture of alumina abrasives and bonding medium containing various amounts of B₂O₃. Microstructural and mechanical examinations have shown that the amount of B₂O₃ present in the starting glass frit determines the ultimate properties of the glass-ceramic bond which can be successfully used in the Al₂O₂/CBN abrasive systems.     

Fabrication of conductive porous alumina (CPA) structurally modified with carbon nanotubes (CNT)

A novel binary porous composite nano-carbon networks (NCNs)/alumina, which is denoted as electrically conductive porous alumina (CPA), was structurally modified by carbon nanotubes (CNT) pre-treated with mixed concentrated acids at 60 °C for 6 h in this study. This conductive ceramics (CCs) was fabricated by combination of gelcasting and high temperature reductive sintering (HTRS) in novel atmosphere. CNT pre-treatment leading to the increased hydrophilicity makes it possible to make uniformly dispersed CNT/alumina slurry. And by HTRS in Ar at 1700 °C for 2 h, well-gelled polymer net-paths in green body prepared by gelcasting technology were totally converted to nano-carbon networks (NCNs) without destruction of CNT. NCN with graphitic crystal structure was evaluated by Raman spectroscopy in sintered ceramic body. Moreover, comparing with as-received CNT, the decreased surface defect of detected composite also supported the further graphitization of CNT via HTRS in Ar instead of burning out. With the aid of field-emission scanning electronic microscopy (FE-SEM) observation, the increased alumina grains in sintered ceramic body CNT/NCN/alumina was valid. Moreover, it was demonstrated that there were three components in this composite, which is carbon filler with two different forms (CNT and NCN) and alumina matrix. And these three components CNT covered with Al₂O₃ particles (Al₂O₃/CNT), NCN and alumina grains (alumina) co-exist in four different situations as follows: (a) Al₂O₃/CNT–alumina co-junction, (b) Al₂O₃/CNT–NCN co-junction, (c) Al₂O₃/CNT–alumina–NCN and (d) Al₂O₃/CNT mesh between alumina boundaries. Furthermore, by comparing with binary composite NCN/alumina (CPA), the increased flexural strength of ternary composite CNT/NCN/alumina (CNT/CPA) up to 38 MPa was attributed to the reinforcement CNT acting as elastic bridge in composite.     

Densification, phase composition, and properties of borosilicate glass composites containing nano-alumina and titania

Five samples of glass/ceramic composites were prepared from borosilicate glasses and both nano-aluminum oxide and nano-titanium oxide. The glass composite samples contain 10, 20, 30, 40, 50 wt.% of alumina and titania mixture. The ratio of Al₂O₃:TiO₂ in the mixture was 1:1. The formation of cristobalite in the glass matrix of low firing glass/ceramic composite substrates limits the efficiency of the ceramic substrate when it is used in circuit boards. In the present study, addition of both alumina and titania to a borosilicate glass as a ceramic filler caused the diffusion of alumina and titania phases (anatase and rutile) constituents into the glass matrix and prevented the formation of a cristobalite. Addition of both the ceramics suppresses cristobalite formation more effectively than one of them used alone and results in lower dielectric constant and thermal expansion coefficients.     

Enhancement of tensile and thermal properties of epoxy nanocomposites through chemical hybridization of carbon nanotubes and alumina

This paper presents the properties of epoxy nanocomposites, prepared using a synthesized hybrid carbon nanotube–alumina (CNT–Al₂O₃) filler, via chemical vapour deposition and a physically mixed CNT–Al₂O₃ filler, at various filler loadings (i.e., 1–5%). The tensile and thermal properties of both nanocomposites were investigated at different weight percentages of filler loading. The CNT–Al₂O₃ hybrid epoxy composites showed higher tensile and thermal properties than the CNT–Al₂O₃ physically mixed epoxy composites. This increase was associated with the homogenous dispersion of CNT–Al₂O₃ particle filler; as observed under a field emission scanning electron microscope. It was demonstrated that the CNT–Al₂O₃ hybrid epoxy composites are capable of increasing tensile strength by up to 30%, giving a tensile modulus of 39%, thermal conductivity of 20%, and a glass transition temperature value of 25%, when compared to a neat epoxy composite.     

Utilization of Chemically Synthesized Fine Powders of SiC/Al2O3 Composites for Sintering

Fine powders of (Al₂O₃)_100–x(SiC)_x (0 ≤ x ≤ 50) composites were prepared by chemical route (named as pyrophoric technique) to achieve a uniform mixture of SiC in an alumina matrix. The chemically synthesized fine SiC/Al₂O₃ composite powders were sintered to form composites at 1450°C which is well below the sintering temperature of SiC. Sintering was performed in an argon atmosphere. Highly dense SiC/Al₂O₃ microstructures were achieved. An improvement in bulk density and hardness has been achieved for SiC/Al₂O₃ composites with 20 wt% of SiC. Hexagonal-shaped grains have been obtained in (Al₂O₃)₅₀(SiC)₅₀ composite with well-connected grain boundaries. The peak position of alumina in SiC/Al₂O₃ composites shifts toward lower wavenumbers in Fourier transform infrared spectroscopy and higher wavenumbers in Raman spectroscopy due to the incorporation of SiC in the composites. The optical band gap decreases with the addition of SiC and the composite behaves more like a semiconductor rather than an insulator. These properties make SiC/Al₂O₃ composites attractive for various industrial applications.     

Fabrication of new porcelain body using nonplastic raw materials by slip casting

New porcelain bodies using only nonplastic raw materials, such as volcanic glass, quartz, alumina and aluminous cement, were fabricated, and their properties were investigated. Green strength increased with increasing Al₂O₃ content at the constant amount of volcanic glass and aluminous cement, caused by the increase of green bulk density with small sized Al₂O₃ addition. The phases in the fired body were glass, -quartz, cristobalite, anorthite and -Al₂O₃. High flexural strength with 10 wt% Al₂O₃ addition was attributed to a strong residual stress induced by the large difference in the thermal expansion coefficient between the glass matrix and the quartz grains, and an additional prestress was induced by Al₂O₃ grains. Higher density and fewer fracture origin were also indicated as potential factors leading to the strengthening effect.     

Mechanical properties and microstructure of Al<Subscript>2</Subscript>O<Subscript>3</Subscript>/mullite composite

An Al₂O₃/5 vol.% mullite composite was synthesized by using reaction sintering of Al₂O₃/0.78 wt.% SiC at 1,600 °C for 2 h in air. The phase analysis of the Al₂O₃/mullite composite was carried out using X-ray diffraction (XRD). There were two kinds of mullite in alumina/mullite composite, namely, 3Al₂O₃·2SiO₂ and Al_5.65Si_0.35O_9.175. The microstructure of the Al₂O₃/mullite composite was investigated using scanning electron microscope (SEM) and transmission electron microscope (TEM). The mechanical properties such as Young’s modulus, Poisson’s ratio, hardness, toughness and strength of the Al₂O₃/mullite composite were investigated. The influence of mullite on the composite is discussed.     

Whiskers of Al2O3 as reinforcement of a powder metallurgical 6061 aluminium matrix composite

An Al-Mg-Si alloy matrix composite reinforced with 10 vol.% of alumina whiskers (Al₂O₃w) has been processed by powder metallurgy and investigated. The Al₂O₃w were produced as single crystal c-axis alpha-alumina fibres at pre-pilot scale via vapour-liquid-solid (VLS) deposition in a cold-wall air-tight furnace with alumina linings. As far as we know, this is the first report of the utilization of whiskers of Al₂O₃ as reinforcing elements for Al alloys. Tensile tests have been performed on the composite at room and high temperatures. Results show that the AA6061 alloy reinforced with the as-produced Al₂O₃ whiskers has remarkably high mechanical properties at room temperature. This is attributed to the high quality of the Al₂O₃ single crystals and to the strong bonding attained between them and the 6061 alloy matrix.     

Fatigue and R-curve behavior of an Al2O3-10vol%Cr3C2 composite

The static and dynamic fatigue properties of an Al₂O₃-10 composite were studied. The R-Curve behavior was determined using the indentation strength in bending (ISB) technique. Results indicated that both alumina and the Al₂O₃-Cr₃C₂ composite exhibit time-dependent slow crack growth under static fatigue test conditions. In addition, the resistance for slow crack growth in the Al₂O₃-Cr₃C₂ composite is higher than that in monolithic alumina. The toughness of alumina was substantially increased and R-curve behavior became evident after the incorporation of Cr₃C₂ particles.     

Low temperature extrusion of 6061 aluminum matrix composite reinforced with SnO2-coated Al18B4O33 whisker

The 6061 aluminum matrix composite reinforced with SnO₂-coated Al₁₈B₄O₃₃ whisker was fabricated by squeeze casting and following by extrusion extruded at elevated temperatures from 300 °C to 400 °C. Optimization of the extruding process, microstructure, texture and mechanical properties of the extruded composites were investigated. The lowest extrusion temperature at which a composite rod with high surface quality was successfully produced was 300 °C. The yield strength of composites is much improved after extrusion, and especially their elongation is increased by 300%. Such big improvements depend on a fact that SnO₂ coating can introduce low-melting-point Sn phase into the interface through an interfacial reaction. The melting of interphase and their surrounding areas is the main reason for the excellent extrusion ability of the composite. Besides, detailed X-ray diffraction analysis of the extruded composite textures reveals the significant effects of extrusion temperatures on their features.     

Phase formation and microstructure during laser sintering and crystallization of a 4.2 MgO·5.0 ZnO·44.1 CaO·26.7 Al<Subscript>2</Subscript>O<Subscript>3</Subscript>·20.0 SiO<Subscript>2</Subscript> glass

In order to produce housings for high-temperature applications, alumina is a highly advantageous material because it has a high chemical durability and withstands high temperatures. If alumina is to be sealed, materials are necessary which have an adapted coefficient of thermal expansion (8.6 × 10^?6 K^?1). If temperature-sensitive components have to be encapsulated, a rapid laser sealing process is highly advantageous. This process requires a glass which can rapidly be crystallized. In this paper, a glass powder with the composition 4.2 MgO·5.0 ZnO·44.1·CaO·26.7 Al₂O₃·20.0 SiO₂ was sintered and subsequently crystallized using a CO₂-laser. As crystalline phases, predominantly a solid solution of akermanite and gehlenite (AGSS) was formed and as phases with minor concentrations Al₂O₃, spinel/gahnite solid solution and ZnO. The AGSS grains have sizes of approximately 5 µm, and Mg and Zn are enriched at the grain boundaries. After sealing at temperatures of 985 and 1135 °C, a similar microstructure and similar grain sizes were observed. The AGSS seems to nucleate at the glass/Al₂O₃ interface but also in the bulk. The AGSS and all other phases do not show a preferred orientation. The resulting coefficients of thermal expansion fit well to that of Al₂O₃.     

Influence of surface modification of alumina on bond strength in Al2O3/Al/Al2O3 joints

The subject of the work was to study the effect of Ti thin film on alumina ceramic on mechanical strength and fracture character of Al₂O₃/Al/Al₂O₃ joints. The joints were formed by liquid state bonding of alumina substrates covered with titanium thin film of 800 nm thickness using Al interlayer of 30μm thickness at temperature of 973 K in a vacuum of 0.2 mPa for 5 min. The bend strength was measured by four–point bending test at room temperature. Scanning and transmission electron microscopy were applied for detailed characterization of interface structure and failure character of fractured joint surfaces. Result analysis has shown that application of the Ti thin film on alumina leads to decrease of bond strength properties of Al₂O₃/Al/Al₂O₃ joints along with the change either of structure and chemistry of interface or of failure character.     

Characterization of metal-supported Al2O3 thin films by scanning electrochemical microscopy

In this paper, physiochemical properties of amorphous alumina thin films, grown by the metal organic chemical vapour deposition process on the surface of platinum (Pt/Al₂O₃) and stainless steel (SS/Al₂O₃), were investigated in aqueous media. The study was performed by the use of scanning electrochemical microscopy (SECM), which allowed obtaining information on uniformity, topography and chemical stability/reactivity of the alumina coatings with high spatial resolution. In particular, the effects due to local acid, base and fluoride ions attack on alumina layers of thickness of about 250 nm (in the Pt/Al₂O₃ sample) and 1000 nm (in the SS/Al₂O₃ sample) were investigated. In the acid and base attack, high concentrations of H₂SO₄ and KOH were electrogenerated locally by the use of a 25 μm diameter platinum microelectrode. The latter was also used as SECM tip to monitor the chemical effect on the alumina layers. It was found that, regardless of the thickness of the film, alumina provided good resistance against local attack of concentrated H₂SO₄; instead, the film dissolved when subjected to KOH attack. The dissolution rate depended on several experimental parameters, such as SECM-tip to substrate distance, electrolysis time and alumina film thickness. The alumina layer proved also relatively poor resistance to etching in 0.1 M NaF solutions.     

Interfaces in nickel aluminide/alumina fibre composites

Metal matrix composites based on the intermetallic alloy Ni₃Al and fibres of Al₂O₃ were fabricated by hot-pressing nickel aluminide powders and alumina fibres. Two matrix alloys were used in this investigation: Ni₃Al microalloyed with boron and Ni₃Al alloyed with 8 at% chromium and smaller amounts of zirconium and boron. The materials were studied using optical and transmission electron microscopy with particular emphasis placed on the characteristics of the matrix-fibre interface. The base Ni₃Al/Al₃O₃ composite displayed no evidence of chemical reaction at the interface, an intimate bond between matrix and fibre was observed, and the material exhibited 10% ductility at room temperature. Composites with the more complex matrix alloy were brittle, a phenomenon attributed to the formation of zirconia particles at the interface.     

Nanostructured AA5005/Al2O3 composite manufactured by anodising and accumulative roll bonding

In this study, nanostructured AA5005/6 vol.-% Al₂O₃ composite manufactured by anodising and accumulative roll bonding (ARB) processes was investigated. The microstructure of the AA5005/Al₂O₃ composite after ninth ARB cycle exhibited a good distribution of alumina reinforcement particles in the AA5005 matrix. It was found that with increasing the number of cycles, the tensile strength of the monolithic and composite samples increased, but their ductility decreased at the first ARB cycle and then increased. The mean grain size of the composite sample after the ninth cycle was 88?nm. The tensile strength of the composite was 3.3 times higher than the initial AA5005 sheet. Observations revealed that the failure mode in the AA5005/Al₂O₃ composite was the shear ductile fracture.     

Metal distribution in alumina/aluminium composites synthesized by directed metal oxidation

The directed oxidation of molten aluminium alloys by vapour phase oxidants can be used to produce Al₂O₃/Al ceramic matrix composites. The toughness of these composites is determined by the amount and the nature of metal distribution in the composite. This paper addresses the problem of understanding the metal distribution in Al₂O₃/Al composites and its dependence on growth temperature. Electrical conductivities and microstructures of Al₂O₃/Al composites synthesized by directed oxidation of Al-5056 alloy are investigated. The high conductivity of the Al₂O₃/Al composite compared to sintered Al₂O₃-4 wt% MgO is shown as a proof of the presence of some continuous metal channels in the composite. The activation energy forthe diffusion of the dominant charge carrier in the oxide matrix is found to be 1.36 eV from the analysis of the conductivity data. Both the amount of metal in the composite and the extent of interconnection of the metal channels decrease with increasing growth temperature. The observed changes in microstructure with temperature can be explained by considering temperature variations of grain boundary energies in alumina and the alumina/aluminium interfacial energy. The metal content of the Al₂O₃/Al composites, prepared by directed oxidation of Al-5056 alloys, can be tailored by the choice of the growth temperature.     

Surface and interface characterization of nanoporous alumina templates produced in oxalic acid and submitted to etching procedures

High purity aluminum (Al) sheets were used to produce ordered nanoporous alumina templates by two step anodization technique using oxalic acid as electrolyte. Electrochemical polishing of Al sheets was performed in order to study the surface roughness influence on the pore roundness of the alumina templates. The templates were submitted to progressive reduction of anodizing voltage (electrochemical etching) to thin the Al₂O₃ barrier layer on the bottom of the pores, and to chemical etching to widen the diameter of the pores. The pore diameter and porosity increase linearly with the chemical etching time, while interpore distance, circularity, pore density and pore distribution do not change. Electropolished Al substrates produce nanoporous Al₂O₃ templates with more circular pores, and the Al₂O₃ barrier layer at the Al₂O₃/Al interfaces is completely removed after the electrochemical and chemical etching processes.     

Herstellung und Prüfung festkörpergeschweißter Keramik-Metall-Verbindungen

Preparation and Testing of Solid-State Bonded Ceramic-to-Metal-Joints Ceramic-to-metal joints were manufactured by solid-state bonding in a R. F.-high-vacuum apparatus. The influence of welding temperature, welding time and welding pressure on the bond strength was investigated for an alumina/niobium-combination consisting of a layered composite ceramic-metal foil-ceramic. As a measure of bond quality the fracture resistance K_ICV was chosen. K_ICV date were obtained by the use of 4-point bend tests and tensile tests. For comparison, data are presented concerning the fracture resistance K_IC of the bulk alumina and the conventional bond strength of the joints. In addition to the Nb/Al₂O₃-data, K_ICV factors are determined for other metal/alumina combinations and for a Zr/Si₃N₄ joint. The present solid-state bonding apparatus was used for the preparation of the specimens. A device for high-temperature bend testing in a high vacuum was constructed. Some data for the high-temperature bond strength of solid-state bonded joints are given.