Characterization of Porous Alumino-Silicate Bonded SiC-Ceramics Prepared by Hand-Pressing and Extrusion Methods

Silicon carbide was mixed with alumina and kaolin to obtain porous alumino-silicate bonded SiC ceramics. Starch was added as sacrificial template. The mixtures were processed by hand-pressing and extrusion method. The effect of firing temperature (1450 ^°C) and the addition of starch on the composition and characteristics of fired specimens were studied. The changes in phase composition and microstructure of fired SiC specimens were followed through x-ray diffraction analysis and scanning electron microscopy, respectively. The sintering parameters and thermal oxidation in air of such specimens were determined. The results indicated that silicon carbide is oxidized during firing into silica which reacted with silica-alumina mixture forming alumino-silicate bonding. Meanwhile, starch burnt out leaving pores inside the specimens. Porous SiC specimens of 1.72 to 1.79 g.cm^?2 bulk density, 40 to 45% open porosity and 250 to 350 N.cm^?2 compressive strength could be obtained by using a mixture of 80 mass% SiC and 20 mass% alumina and kaolin as starting materials. The properties of porous SiC specimens depend on the type and amount of used starch. The extrusion method is favorable for preparing porous SiC articles of homogeneous microstructure and good properties.     

The Manipulation and Alignment of Silicon Carbide Whiskers for Gallium Nitride Epitaxial Growth

As a substrate candidate for low‐cost III‐nitride thin film growth, 3C–SiC whiskers are employed and manipulated in this work. The alignment of the whiskers is achieved on a patterned 3M Vikuiti^? Brightness Enhancement Film surface. The degree of whisker alignment using this approach is higher than the whiskers lined up by extrusion methods according to X‐ray diffraction (XRD) analysis. The aligned whiskers are transferred from the 3M film and embedded into an alumina matrix by tape casting. A self‐regulating sintering technique for SiC whiskers is used to protect the whiskers from being oxidized in air during sintering at 1600°C. The aligned whiskers are rigidly embedded in the alumina matrix as shown in scanning electron microscopy (SEM) images and energy‐dispersive X‐ray spectrometry energy mapping images. GaN thin films grown by a low‐cost sputtering process on Alumina/SiC as well as Si and SiC as reference materials are characterized by XRD and SEM.     

The relationship between microstructure,fracture and abrasive wear in Al2O3/SiC nanocomposites and microcomposites containing 5 and 10% SiC

Alumina/SiC nanocomposites are much more resistant to severe wear than monolithic alumina. In order to clarify the mechanisms responsible for these improvements, alumina and alumina/SiC nanocomposites with 5 and 10 vol.% SiC and various alumina grain sizes were fabricated. For comparison, a 10 vol.% SiC “microcomposite” was also fabricated using 3 μm SiC particles. The extent of cracking beneath hardness indentations was examined and the specimens were tested in abrasive wear. Quantitative surface fractography of the worn surfaces was carried out. The wear properties depended strongly on the grain size in pure alumina, but were independent of the alumina grain size in the nanocomposites. This is consistent with the idea that much of the improvement in wear resistance when SiC is added to alumina stems from a reduction in the size of the individual pullouts owing to the accompanying change in fracture mode. In addition, crack initiation by plastic deformation during abrasion and indentation was found to be strongly inhibited when 10 vol.% nanosized SiC was added to alumina. The addition of 3 μm “micro-sized” SiC did not have the same effect. The ability of fine SiC particles to suppress cracking is attributed to the blocking of twins and dislocation pileups by intragranular SiC nanoparticles. This reduces the length of the twins or pileups and hence their ability to nucleate microcracks.     

Highly resistive SiC ceramics sintered with Al2O3-AlN-Y2O3 additions

A polycrystalline SiC ceramic prepared by pressureless sintering of α-SiC powders with 3 vol% Al₂O₃-AlN-Y₂O₃ additives in an argon atmosphere exhibited a high electrical resistivity of ~10¹³ Ω cm at room temperature. X-ray diffraction revealed that the SiC ceramics consisted mainly of 6H- and 4H-SiC polytypes. Scanning electron microscopy and high resolution transmission electron microscopy investigations showed that the SiC specimen contained micron-sized grains surrounded by an amorphous Al-Y-Si-O-C-N film with a thickness of ~4.85 nm. The thick boundary film between the grains contributed to the high resistivity of the SiC ceramic.     

Electrical conductivity and thermal properties of spark plasma sintered Al2O3-SiC-CNT hybrid nanocomposites

In this study, we report the electrical conductivity and thermal properties of Al₂O₃-SiC-CNT hybrid nanocomposites processed via ball milling (BM) and spark plasma sintering (SPS). The initial powders and consolidated samples were characterized using transmission electron microscopy (TEM) and field emission scanning electron microscopy (FE-SEM), respectively. A multifunction calibrator and a high-resolution digital multimeter were used to measure the electrical conductivity. The thermal properties were measured using a thermal constants analyser. The SiC and CNT-reinforced alumina hybrid nanocomposites exhibited a significant increase in their room-temperature electrical conductivity, which made them suitable for electrical discharge machining. The Al₂O₃-5SiC-2CNTs had a high electrical conductivity value of 8.85 S/m compared to a low value of 6.87×10⁻¹⁰ S/m for the monolithic alumina. The addition of SiC and CNTs to alumina decreased its room-temperature thermal properties. The increase in temperature resulted in a decrease in the thermal conductivity and thermal diffusivity but an increase in the specific heat of the monolithic alumina and the hybrid nanocomposites. These properties were correlated with the microstructure, and possible transport mechanisms were discussed.     

Effect of Oxidation on Crack Deflection in SiC/Al2O3 Laminated Ceramic Composites

Laminated composites consisting of SiC and a thin porous alumina interphase were exposed to air at 500°C to produce a persistent, nearly uniform oxidation product layer. Crack deflection at the interface was then studied using a four-point bend testing procedure and interfacial fracture resistances were found to decrease with increasing oxidation times. Electron microscopy observations of the fractured interface show a complex multi-phase microstructure. These results show that oxidation can produce a sufficiently weak interface in a SiC-porous alumina interphase composite, in contrast to most other SiC composites where interface oxidation produces a strongly bonded interface which inhibits crack deflection.     

Raman/Cr3+ fluorescence mapping of a melt-grown Al2O3/GdAlO3 eutectic

The paper reports on the Raman/fluorescence study of a melt-grown Al₂O₃/GdAlO₃ eutectic composite. Raman bands from the α-alumina and gadolinium perovskite phases identified by X-ray diffraction were systematically observed together in the optically visible domains, even when the latter were much larger than the Raman probe. This suggests a more complex interlocking pattern than appearing on SEM or optical microscopy images. The polarization of alumina and GdAlO₃ Raman bands evidenced the preferential orientation of Al₂O₃ phase with respect to the sample growth direction, in agreement with TEM results. In addition, the position of chromium impurity fluorescence bands was used to map the residual stress in alumina phase. It is a compression in the 200–300 MPa range.     

High resolution optical microprobe investigation of surface grinding stresses in Al2O3 and Al2O3/SiC nanocomposites

It has previously been suggested that Al₂O₃/SiC nanocomposites develop higher surface residual stresses than Al₂O₃ on grinding and polishing. In this work, high spatial resolution measurements of residual stresses in ground surfaces of alumina and nanocomposites were made by Cr³⁺ fluorescence microspectroscopy. The residual stresses from grinding were highly inhomogeneous in alumina and 2 vol.% SiC nanocomposites, with stresses ranging from ～ ?2 GPa within the plastically deformed surface layers to ～ +0.8 GPa in the material beneath them. Out of plane tensile stresses were also present. The stresses were much more uniform in 5 and 10 vol% SiC nanocomposites; no significant tensile stresses were present and the compressive stresses in the surface were ～ ?2.7 GPa. The depth and extent of plastic deformation were similar in all the materials (depth ～ 0.7–0.85 μm); the greater uniformity and compressive stress in the nanocomposites with 5 and 10 vol% SiC was primarily a consequence of the lack of surface fracture and pullout during grinding. The results help to explain the improved strength and resistance to severe wear of the nanocomposites.     

Visible-light photocatalytic activity of SiC hollow spheres prepared by a vapor–solid reaction of carbon spheres and silicon monoxide

SiC hollow spheres are obtained by a vapor–solid reaction using carbon spheres as templates. The prepared SiC hollow spheres are characterized by X-ray diffraction, scanning electron microscopy, nitrogen adsorption, and UV–vis diffuse reflectance spectra. The visible-light photocatalytic activity is evaluated by photocatalytic decomposition of the methylene blue in aqueous solution. Results show that the diameter of SiC hollow spheres ranges from 200 to 300 nm and the shell thickness is about 50 nm. The SiC hollow spheres have a high surface area of 83.5 m²/g and exhibit a mesoporous structure characteristic. The photo-response of the SiC hollow spheres expand to visible-light region with band gap energy of 2.15 eV. The SiC hollow spheres exhibit a significantly enhanced photocatalytic activity due to their high surface area as well as large light-harvesting efficiencies.     

Microstress in Reaction‐Bonded SiC from Crystallization Expansion of Silicon

Microstress in reaction‐bonded silicon carbide (RBSiC) has been measured using piezo‐Raman spectroscopy. Compressive microstresses as high as 2 GPa exist in the silicon phase and tensile microstresses as high as 2.3 GPa exist in the SiC phase of RBSiC. This is much larger than expected for thermoelastic microstress from coefficient of thermal expansion mismatch would provide. Instead the microstresses arise from the crystallization of liquid silicon. During the reaction bonding process, not all of the silicon reacts to form SiC and there is liquid free silicon. The phase transformation of the free silicon from liquid to solid has a large volume expansion, which results in large residual microstress within the silicon and SiC phases of RBSiC.     

Mechanical Behavior of Alumina Reinforced with Carbon-Coated Silicon Carbide Whiskers

SiC whiskers with 0, 20, and 50 Å carbon coatings were incorporated into an alumina matrix to modify residual thermal stress and interfacial bonding. Composites were characterized using triaxial X-ray diffraction for residual stress determination and electron microscopy to explore interfacial chemistry. Fracture toughness and R -curve behavior were examined for short and long crack lengths. Uncoated SiC whiskers optimized strength, fracture toughness, and R -curve behavior of these composites. A graphite interphase at the whisker/matrix interface decreased contributions to crack bridging without promoting additional toughening by whisker pullout.     

Electrical conductivity of spark plasma sintered Al2O3–SiC and Al2O3-carbon nanotube nanocomposites

The electrical conductivity of alumina-silicon carbide (Al₂O₃–SiC) and alumina-multiwalled carbon nanotube (Al₂O₃-MWCNT) nanocomposites prepared by sonication and ball milling and then consolidated by spark plasma sintering (SPS) is reported. The effects of the nanophase (SiC and MWCNTs) and SPS processing temperature on the densification, microstructure, and functional properties were studied. The microstructure of the fabricated nanocomposites was investigated using field-emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM). The phase evolution was determined using X-ray diffraction (XRD). The room-temperature direct current (DC) electrical conductivity of the monolithic alumina and nanocomposites was determined using the four-point probe technique. The EDS mapping results showed a homogenous distribution of the nanophases (SiC and MWCNTs) in the corresponding alumina matrix. The room-temperature DC electrical conductivity of monolithic alumina was measured to be 6.78 × 10⁻¹⁰ S/m, while the maximum electrical conductivities of the alumina-10 wt%SiC and alumina-2wt%MWCNT samples were 2.65 × 10⁻⁵ S/m and 101.118 S/m, respectively. The electrical conductivity increased with increasing nanophase concentration and SPS temperature. The mechanism of electrical conduction and the disparity in the electrical performance of the two investigated nanocomposite systems (alumina-SiC and alumina-MWCNT) are clearly described.     

Confocal fluorescence microscopy in alumina-based ceramics: Where does the signal come from?

Confocal Cr³⁺ fluorescence microscopy is an ideal technique for investigating residual stresses in alumina-based ceramics. Due to their transparency, however, it is important to understand where the collected signal comes from by characterising the probe response function (PRF). Here, a PRF is proposed that captures all the relevant physical effects, including a newly identified consequence of scattering by pores and grain boundaries. The new PRF describes the response of a range of alumina-based ceramics to depth scanning in a high resolution confocal fluorescence microscope in a manner that balances physical significance with the accuracy of empirical fitting. The results showed that measurements could be made deep within single crystals of sapphire and ruby, although refraction degraded the depth resolution from about 3 μm at the surface to 25 μm at a depth of 500 μm. Scattering and absorption limited the depth to which polycrystalline alumina could be probed to ～15 μm. This was further reduced to ～4 μm for an alumina–10 vol.% SiC nanocomposite. However, the absorption increased the accuracy of near surface measurements in these materials by preventing contamination from subsurface fluorescence.     

Synthesis and characterization of monolithic carbon/silicon carbide composite aerogels

Resorcinol–formaldehyde/silica composite (RF/SiO₂) aerogels were synthesized using sol–gel process followed by supercritical CO₂ drying. Monolithic carbon/silicon carbide composite (C/SiC) aerogels were formed from RF/SiO₂ aerogels after carbothermal reduction. X-ray diffraction and transmission electron microscopy demonstrate that β-SiC was obtained after carbothermal reduction. Scanning electron microscopy and nitrogen adsorption/desorption reveal that the as-prepared C/SiC aerogels are typical mesoporous materials. The pore structural properties were measured by nitrogen adsorption/desorption analysis. The resulting C/SiC aerogels possess a BET surface area of 564 m²/g, a porosity of 95.1 % and a pore volume of 2.59 cm³/g. The mass fraction of SiC in C/SiC aerogels is 31 %.     

Crystallization of SiC and its effects on microstructure,hardness and toughness in TaC/SiC multilayer films

A series of TaC/SiC multilayer films with different SiC thicknesses (t_SiC) have been prepared by magnetron sputtering and their microstructure, hardness and toughness investigated by X-ray diffraction (XRD), transmission electron microscopy (TEM), atomic force microscopy (AFM), scanning electron microscopy (SEM) and nanoindentation. Results show that SiC crystallized and grew coherently with TaC layers at low t_SiC (≤ 0.8 nm), resulting from the template effect of TaC layers. Maximum hardness and toughness of 46.06 GPa and 4.21 MPa m^1/2 were achieved at t_SiC = 0.8 nm with good coherent interface. With further increasing of t_SiC, SiC layers partially transformed to an amorphous structure and gradually lost their coherent interface, leading to a rapid drop in hardness and toughness. The crystallization of SiC layers and the coherent growth are required to achieve superhardness and high toughness in the TaC/SiC multilayers.     

Effects of residual stress and intragranular particles on mechanical properties of hot-pressed Al2O3/SiC ceramic composites

Al₂O₃/SiC ceramic composites with different SiC contents have been prepared by powder metallurgy at 1600 °C for 120 min at 30 MPa pressure. The effect of second phase particles on the microstructure and mechanical properties of composites have been studied. The results show that SiC particle has a significant impact on the matrix subjected to residual stress, and on the microstructure of the composites as well. The average grain size of alumina matrix decreases as the SiC particle content increases. Simultaneously, it has been found that the mechanical properties of the material are significantly enhanced in comparison with monolithic Al₂O₃. The highest strength and toughness are obtained when the SiC content is 15 vol%, and the values are 1237 MPa and 5.68 MPa m^1/2, respectively. The mechanisms of strengthening and toughening have been discussed.     

Phase Evolution,Microstructure, and Mechanical Properties of Alumina–Mullite–Zirconia Composites Prepared by Iranian Andalusite

This paper investigates the effects of Iranian andalusite and short milling times on alumina–mullite–zirconia composites. Andalusite powder was added at 0, 2.5, 5, and 10 wt% to an alumina–zircon mixture and the raw materials were milled for 1 or 3 h. The sintering of samples was carried out at the temperatures of 1550°C, 1600°C, and 1650°C for 3 h. Microstructural changes, phase composition, physical properties, and mechanical strength of the sintered composites were characterized by scanning electron microscopy, X‐ray diffraction, density, and strength measurement tests. Results show that andalusite promoted the decomposition of zircon and accelerated the reaction sintering of alumina–zircon, which leads to the formation of much more mullite phase and improvements to the composites’ thermal shock resistance up to about 50%.     

Creep Behavior of a SiC-Whisker-Reinforced Alumina

Creep tests in four-point flexure loading configuration in air employing applied stresses of 37 to 300 MPa at temperatures of 1200°, 1300°, and 1400°C were performed on 20-vol%-SiC-whisker-reinforced alumina and unreinforced single-phase polycrystalline alumina. The creep rate of polycrystalline alumina was significantly reduced through the addition of SiC whiskers, although strain to failure was lower. Transmission and scanning electron microscopy results suggest that substantial increase in the creep resistance in flexure of alumina composites originates from the retardation of grain-boundary sliding by the SiC whiskers.     

Fabrication of cobalt nanowires from mixture of 1-ethyl-3-methylimidazolium chloride ionic liquid and ethylene glycol using porous anodic alumina template

Porous anodic alumina template is synthesized by electrochemical anodization of aluminum and used to grow cobalt nanowires. The cobalt nanowires produced by direct current electrodeposition are characterized by field emission scanning electron microscopy, transmission electron microscopy, X-ray diffraction and physical property measurement system. Test results indicate that the average diameter of cobalt nanowires is about 45 nm, which is generally the same as the pore diameter of porous anodic alumina template, and the cobalt nanowires electrodeposited from mixture of 1-ethyl-3-methylimidazolium chloride ionic liquid and ethylene glycol have a smoother surface and better magnetic properties than cobalt nanowires electrodeposited from aqueous solution, and they show a better squareness. Therefore it can be concluded that the cobalt nanowires electrodeposited from mixture of 1-ethyl-3-methylimidazolium chloride ionic liquid and ethylene glycol using porous anodic alumina template can be used as a perpendicular magnetic recording film.     

Microscopic and Spectroscopic Characterization of Stacking‐Sequence Disordered SiC

Nanometric silicon carbide (SiC) powder (~5 nm) with a stacking‐sequence disordered structure (SD‐SiC), synthesized from elemental powders of Si and C, was investigated by microscopic and several spectroscopic methods. The structure of SD‐SiC was characterized by transmission electron microscopy (TEM), ¹³C, and ²⁹Si‐NMR, and by infrared (IR), Raman, and X‐ray photoelectron spectroscopy (XPS) methods. TEM characterizations showed relatively large deviations of the lattice parameters in the as‐synthesized SiC, indicative of the presence of stacking‐sequence disorder. IR analysis showed a weaker Si‐C bond in the SD‐SiC than in the 3C‐SiC. XPS determinations showed that C and Si in SD‐SiC are similar to those in 3C‐SiC. Broader peaks of ²⁹Si and ¹³C MAS‐NMR also indicate that the structure of SD‐SiC is different from that of 3C‐SiC. Raman spectroscopy exhibited activities for the crystalline polytypes and the amorphous of SiC but lack of them for the SD‐SiC. The inactivity of Raman spectroscopy for the SD‐SiC along with large deviation of the lattice constant and the extremely broad X‐ray diffraction peaks would indicate that SD‐SiC is a possible intermediate state between conventional polytype SiC and amorphous SiC, that is, a possible new type of SiC.