Microstructure and mechanical properties of Al2O3–YSZ spherical polycrystalline composites

The mechanical behavior and microstructure of highly densified, spherically shaped, polycrystalline Al₂O₃–YSZ composites, processed from pseudoboehmite powders by sol–gel is reported here. Processing was carried out by combining nanometric sized α-Al₂O₃ (120 nm) seeds and YSZ particles of tetragonal structure. The YSZ particles were homogeneously distributed in a coarse-grained matrix of alumina, both inside grains and along grain boundaries. Fracture surfaces, achieved by impact tests showed toughening effects of the zirconia particles. The tetragonality of the YSZ phase stability even after fracture events and fracture toughness measurements by Vickers indentation, where the crack tip interacts with YSZ particles, are all provided and discussed. The local mechanical properties, such as elastic modulus, indentation hardness and the onset of plastic deformation or fracture contact pressure of both YSZ particles and the Al₂O₃ matrix were quantified by nanoindentation. Evidence of coercive contact pressure was observed in YSZ from indentation stress–strain curves.     

Microstructure and mechanical properties of multi-walled carbon nanotubes containing Al2O3–C refractories with addition of polycarbosilane

Carbon nanotubes (CNTs) are a promising reinforcement for fabricating Al₂O₃–C refractories. However, CNTs are prone to agglomerate or react with antioxidants or reactive gaseous phases such as Al (g), Si (g) and SiO (g), etc. at high temperatures. To overcome the problems above, polycarbosilane (PCS) and multi-walled carbon nanotubes (MWCNTs) were firstly mixed with micro-alumina powder in a liquid medium and then incorporated into Al₂O₃–C refractories. Then the microstructure and mechanical properties of Al₂O₃–C refractories fired in the temperature range from 800 °C to 1400 °C were investigated in this work. The results showed that the MWCNTs were well dispersed in the specimens with addition of PCS in contrast to the specimens without PCS due to the PCS adsorption on the surface of MWCNTs during the mixing process. And the mechanical properties, such as cold modulus of rupture (CMOR), flexural modulus (FM), forces and displacements of Al₂O₃–C refractories with PCS were much higher than those without PCS, which was attributed to more homogeneous dispersion of MWCNTs, more residual MWCNTs as well as different morphologies of ceramic whiskers. Meanwhile, the oxidation resistance of Al₂O₃–C refractories with PCS was improved greatly, which was supposed that the in situ formed SiC_xO_y coating prevented the oxidation of MWCNTs to some extent.     

Rietveld analysis and mechanical properties of in situ formed La-β-Al2O3/Al2O3 composites prepared by sol-gel method

In this work, the crystal evolution of α-Al₂O₃ composites reinforced with LBA platelets were monitored by XRD Rietveld. In addition, the mechanical properties of totally densified specimens were researched by Vickers and Knoop indentations. These composite materials were prepared by a sol-gel process from alumina seeded boehmite sol and lanthanum nitrate. X-ray diffraction data have been studied by Rietveld refinements and line profile analyses, paying attention to the LBA formation, the evolution of vol%, and crystallite size of the different phases. It has been observed that the appearance of the LBA phase happens at a lower temperature than in samples prepared by a conventional solid state reaction. Indentation tests revealed that the presence of LBA microplatelets in the sol-gel samples leads to a significant increase of their indentation fracture resistance, in comparison to the conventional samples.     

Effects of CNTs content on microstructure and mechanical properties of Cnt/α-Al2O3 and Cnt-Csf/α-Al2O3 composites

In this work, CNTs and short carbon fiber reinforced α-Al₂O₃ matrix composites (i.e., C_nt/α-Al₂O₃ and C_nt-C_sf/α-Al₂O₃) were prepared by sol-gel dispersing method followed by hot pressing process. Effects of CNTs content on the mechanical properties of C_nt/α-Al₂O₃ and C_nt-C_sf/α-Al₂O₃ composites were investigated and the inter- and transgranular fracture mechanisms in C_nt-C_sf/α-Al₂O₃ composites were analyzed. The hardness and relative density of C_nt/α-Al₂O₃ and C_nt-C_sf/α-Al₂O₃ composites slightly decrease as CNTs content increases. The flexural strength and fracture toughness monotonically increase with the increase in C_nt content for both C_nt/α-Al₂O₃ and C_nt-C_sf/α-Al₂O₃ composites. Addition of C_sf and CNTs into α-Al₂O₃ matrix results in a bimodal grain size microstructure of C_nt-C_sf/α-Al₂O₃ composites, which accounts for the unique fractograph and the enhanced toughness of C_nt-C_f/α-Al₂O₃ composites. The flexural strength and fracture toughness of C_sf5-nt06 composite are 465 MPa and 7.08 MPa/m², 37% and 13% higher than that of C_nt06, and 42% and 34% higher than that of C_sf5, respectively.     

Microwave hybrid sintering of Al2O3 and Al2O3–ZrO2 composites,and effects of ZrO2 crystal structure on mechanical properties,thermal properties,and sintering kinetics

Structural ceramics such as Al₂O₃ and Al₂O₃–ZrO₂ composites are widely used in harsh environment applications. The conventional sintering process for fabrication of these ceramics is time-consuming method that requires large amount of energy. Microwave sintering is a novel way to resolve this problem. However, to date, very limited research has been carried out to study the effects of different ZrO₂ crystal structures on Al₂O₃–ZrO₂ composites, especially on the sintering kinetics, when fabricated by microwave sintering.The microwave hybrid sintering of Al₂O₃ and Al₂O₃–ZrO₂ composites was performed in this study. Tetragonal zirconia and cubic zirconia were used as two different reinforcements for an α–alumina matrix, and the mechanical and thermal properties were studied. It was found that Al₂O₃ experienced a remarkable increase in fracture toughness of up to 42% when t-ZrO₂ was added. Al₂O₃–c-ZrO₂ also showed increased fracture toughness. The sintering kinetics were also thoroughly investigated, and the average activation energy values for the intermediate stage of sintering were estimated to be 246 ± 11 kJ/mol for pure Al₂O₃, 319 ± 71 kJ/mol for Al₂O₃–c-ZrO₂, and 342 ± 77 kJ/mol for Al₂O₃–t-ZrO₂. These values indicated that the activation energy was increased by the addition of either type of ZrO₂, with the highest value shown by Al₂O₃–t-ZrO₂.     

Microstructure,mechanical properties and machining performance of spark plasma sintered Al2O3–ZrO2–TiCN nanocomposites

The effect of addition of nanocrystalline ZrO₂ and TiCN to ultrafine Al₂O₃ on mechanical properties and microstructure of the composites developed by spark plasma sintering (SPS) was investigated. The distribution of the nanoparticles was dependent on their overall concentration. Maximum hardness (21 GPa) and indentation toughness (5.5 MPa m^1/2) was obtained with 23 vol% nanoparticles, which was considered as the optimum composition. The Zener pinning criteria were also satisfied at this composition with grain size of the restraining nanoparticles ～63–65 nm. Hardness of the composites follows the rule of mixtures; crack deflection and crack arrest by nanoparticles at grain boundaries along with mixed fracture mode led to high toughness in the nanocomposites. Cutting tool inserts were developed by SPS with the optimized composition and their machining performance was compared with commercial alumina based inserts. Increased toughness in the nanocomposite inserts reflects in the machining performance as the tool life improves drastically compared to that of the commercial inserts at high cutting speeds ≥500 m min^?1. This was attributed to differences in their failure modes; the commercial inserts fail catastrophically by fracture due to their low toughness whereas the nanocomposite inserts reach the tool failure criteria by crater wear at all machining conditions.     

Effect of adding Y2O3 on structural and mechanical properties of Al2O3–ZrO2 ceramics

The effects of adding 1–8 wt% Y₂O₃ on phase formation and fracture toughness of Al₂O₃–xZrO₂–Y₂O₃(AZY) ceramics were studied. Phase formations of the samples were characterized by the X-ray diffraction (XRD) technique. It was found that the major phase was rhombohedral-Al₂O₃, while the minor phase consisted of the monoclinic-ZrO₂, tetragonal-ZrO₂ and monoclinic-Y₂O₃. It was found that Y₂O₃ contents did not clearly influence grain shape of AZY ceramics. The results obtained from the microhardness test could be used to evaluate the fracture toughness. It was found that the smaller grains had high fracture toughness. The maximum fracture toughness of 4.827 MPa m^1/2 was obtained from 4 wt% Y₂O₃. Refinement of lattice parameters using Rietveld analysis revealed the quantitative phases of AZY ceramics. This shows that under adding Y₂O₃ conditions the proportion of tetragonal-ZrO₂ phase plays an important role for the mechanical properties of AZY ceramics.     

The effects of the addition of tetragonal-ZrO2 on the mechanical properties of MgAl2O4 – ZrO2 composites

The effects of the addition of tetragonal 3mol% Y₂O₃ – ZrO₂ into a MgAl₂O₄ spinel matrix were investigated. MgAl₂O₄ spinel's lacking mechanical properties prevent further utilization in many structural and refractory applications even though it has excellent chemical and thermal stability. The addition of tetragonal-ZrO₂ was observed to improve the hardness, fracture toughness and biaxial flexural strength of MgAl₂O₄ materials. Moreover, the additions of 3mol% Y₂O₃ – ZrO₂ resulted in a reduction of the mean grain size.     

Optimization of microstructure and mechanical properties of oscillatory pressure sintered ZrO2–Al2O3-SiCp ceramics

Zirconia ceramic is a significant structural material, but its use under some extreme circumstances is limited by its mechanical properties. In this work, SiC particles (SiCp) were added into alumina toughened zirconia ceramics to prepare ZrO₂–Al₂O₃-SiCp ceramics with high performance by using oscillatory pressure sintering (OPS). Results showed that the best OPS temperature of 1600 °C was obtained, and the optimal SiCp particle size and content were 200 nm and 10 vol% respectively. Under these conditions, the specimen exhibited higher mechanical properties including Vickers hardness of 15.43 GPa, bending strength of 1162 MPa and fracture toughness of 6.36 MPa m^1/2. Moreover, it was found that the atomic matching between ZrO₂/SiCp, Al₂O₃/SiCp, and ZrO₂/Al₂O₃ was much higher, showing the coherent interface relationship. Therefore, it was favorable for enhanced mechanical properties of as-prepared ZrO₂–Al₂O₃-SiCp ceramics.     

Pressure-less joining of SiCf/SiC composites by Y2O3–Al2O3–SiO2 glass: Microstructure and properties

In this study, Y₂O₃–Al₂O₃–SiO₂ (YAS) glass was prepared from Y₂O₃, Al₂O₃, and SiO₂ micron powders. Thermal expansion coefficient of as-obtained YAS glass was about 3.9 × 10⁻⁶, matching-well with that of SiC_f/SiC composites. SiC_f/SiC composites were then brazed under pressure-less state by YAS glass and effects of brazing temperature on microstructures and properties of resulting joints were investigated. The results showed that glass powder in brazed seam sintered and precipitated yttrium disilicate, cristobalite, and mullite crystals after heat treatment. With the increase in temperature, joint layer gradually densified and got tightly bonded to SiC_f/SiC composite. The optimal brazing parameter was recorded as 1400 °C/30 min and shear strength of the joint was 51.7 MPa. Formation mechanism of glass-ceramic joints was proposed based on combined analysis of microstructure and fracture morphology of joints brazed at different temperatures. Thermal shock resistance testing of joints was also carried out, which depicted decline in shear strength with the increase of thermal shock times. The strength of the joint after three successive thermal shock cycles at 1200 °C was 35.6 MPa, equivalent to 69% of that without thermal shock.     

Simultaneous enhancement of mechanical and microwave absorption properties with a novel in-situ synthesis α-Al2O3 fillers for SiCf/SiC composites

The Al and H₃BO₃ mixed powder was introduced into the PCS/Xylene precursor solution as in-situ synthesis α-Al₂O₃ filler by precursor infiltration and pyrolysis (PIP) method. The in-situ synthesis filler can effectively decrease the open porosity of SiC_f/SiC composites and give rise to multiple scattering of microwave and dipolar polarization. Therefore, the mechanical and microwave absorption properties of SiC_f/SiC composites can be simultaneously enhanced. The effects of in-situ synthesis filler on the morphologies, flexure strength and reflection loss values of SiC_f/SiC composites were investigated. With 2 wt% in-situ synthesis filler, the flexure strength of SiC_f/SiC composite was 305 MPa and the maximum reflection loss (RL_m) can reach ? 54.68 dB with the effective absorption band (EAB) of 3.51 GHz in the X band. With 5 wt% in-situ synthesis filler, the flexure strength of SiC_f/SiC composite was 207 MPa and the RL_m was ? 30.91 dB. Due to the inefficient infiltration process, the RL_m of SiC_f/SiC composites with 10 wt% in-situ synthesis filler was only ? 27.36 dB. Nevertheless, the flexure strength of that composite was 259 MPa, owing to the dense matrix. Additionally, the flexure strength of SiC_f/SiC composite without filler was 148 MPa and the RL_m was ? 26.40 dB.     

Microstructure and mechanical properties of Al2O3/Cu joints brazed with Ag–Cu–Ti+Zn composite fillers

In this study, Al₂O₃ ceramic and Cu bars were brazed with newly designed Ag–Cu–Ti(ABA)+Zn composite fillers. Systematic analysis of the microstructure of the brazed joints indicated that the volatilization of Zn atoms during the brazing process could promote the spreading of liquid brazing fillers on the surface of the Al₂O₃ ceramic, resulting in a uniform dendritic interfacial structure. The typical interfacial structure was an Al₂O₃/TiO/(Cu, Al)₃Ti₃O+Ag(s, s)/Cu interface. Notably, the tensile strength was improved to 20.89 MPa for Al₂O₃/Cu joint brazed with ABA+Zn composite fillers at 900 °C for 20 min, approximately 67.6% higher than the sample brazed without Zn foil. In this case, the fracture model was straight and sharp-angled inside the Al₂O₃ ceramic. In addition, the joint strength decreased with increased brazing temperatures from 900 to 940 °C.     

Fabrication and mechanical properties of Al2O3–TiC ceramic composites synergistically reinforced with multi-walled carbon nanotubes and graphene nanoplates

In this study, Al₂O₃–TiC composites synergistically reinforced with multi-walled carbon nanotubes (MWCNTs) and graphene nanoplates (GNPs) were prepared via spark plasma sintering (SPS). The effects of the MWCNT and GNP contents on the phase composition, mechanical properties, fracture mode, and toughening mechanism of the composites were systematically investigated. The experimental results indicated that the composite grains became more refined with the addition of MWCNTs and GNPs. The nanocomposites presented high compactness and excellent mechanical properties. The composite with 0.8 wt% MWCNTs and 0.2 wt% GNPs presented the best properties of all analysed specimens, and its relative density, hardness, and fracture toughness were 97.3%, 18.38 ± 0.6 GPa, and 9.40 ± 1.6 MPa m^1/2, respectively. The crack deflection, bridging, branching, and drawing effects of MWCNTs and GNPs were the main toughening mechanisms of Al₂O₃–TiC composites synergistically reinforced with MWCNTs and GNPs.     

Microstructure and mechanical properties of Al2O3 ceramic and TiAl alloy joints brazed with Ag–Cu–Ti filler metal

Al₂O₃ ceramic was reliably joined to TiAl alloy by active brazing using Ag–Cu–Ti filler metal, and the effects of brazing temperature, holding time, and Ti content on the microstructure and mechanical properties of Al₂O₃/TiAl joints were investigated. The typical interfacial microstructure of joints brazed at 880 °C for 10 min was Al₂O₃/Ti₃(Cu,Al)₃O/Ag(s.s)+AlCu₂Ti+Ti(Cu,Al)+Cu(s.s)/AlCu₂Ti+AlCuTi/TiAl alloy. With increasing brazing temperature and time, the thickness of the Ti₃(Cu,Al)₃O reaction layer increased, and the blocky AlCu₂Ti compounds aggregated and grew gradually. The Ti dissolved from the TiAl substrate was sufficient to react with Al₂O₃ ceramic to form a thin Ti₃(Cu,Al)₃O layer when Ag–Cu eutectic alloy was used, but the dissolution of TiAl alloy was inhibited with an increase in Ti content in the brazing filler. Ti and Al dissolved from the TiAl alloy had a strong influence on the microstructural evolution of the Al₂O₃/TiAl joints, and the mechanism is discussed. The maximum shear strength was 94 MPa when the joints were brazed with commercial Ag–Cu–Ti filler metal, while it reached 102 MPa for the joint brazed with Ag–Cu+2 wt% TiH₂ at 880 °C for 10 min. Fractures propagated primarily in the Al₂O₃ substrate and partially along the reaction layer.     

Particle occlusion and mechanical properties of Ni–Al2O3 nanocomposites

Polycrystalline alumina, doped with MgO below the solubility limit, was reinforced with sub-micron particles of Ni by infiltration of Ni-nitrate into fired alumina green bodies, followed by reduction and sintering. The Ni particle size and location were monitored both after reduction and after sintering by transmission electron microscopy. Particle occlusion was found to increase with sintering time and temperature, and is correlated with experimentally detected Mg segregation to the Ni–alumina interfaces, resulting in partial depletion of Mg at the alumina grain boundaries and thus their increased mobility. Occlusion of Ni particles reduces the fracture strength and Weibull modulus of the composites, indicating that particle location is a key microstructural parameter for reaching high fracture strengths, and that this can be controlled via grain boundary and interface adsorption.     

Microstructure and properties of SiCf/SiC composite joints with CaO–Y2O3–Al2O3–SiO2 interlayer

Using CaO, Y₂O₃, Al₂O₃, and SiO₂ micron-powders as raw materials, CaO–Y₂O₃–Al₂O₃–SiO₂ (CYAS) glass was prepared using water cooling method. The coefficient of thermal expansion (CTE) of CYAS glass was found to be 4.3 × 10^?6/K, which was similar to that of SiC_f/SiC composites. The glass transition temperature of CYAS glass was determined to be 723.1 °C. With the increase of temperature, CYAS glass powder exhibited crystallization and sintering behaviors. Below 1300 °C, yttrium disilicate, mullite and cristobalite crystals gradually precipitated out. However, above 1300 °C, the crystals started diminishing, eventually disappearing after heat treatment at 1400 °C. CYAS glass powder was used to join SiC_f/SiC composites. The results showed that the joint gradually densified as brazing temperature increased, while the phase in the interlayer was consistent with that of glass powder heated at the same temperature. The holding time had little effect on phase composition of the joint, while longer holding time was more beneficial to the elimination of residual bubbles in the interlayer and promoted the infiltration of glass solder into SiC_f/SiC composites. The joint brazed at 1400 °C/30 min was dense and defect-free with the highest shear strength of about 57.1 MPa.     

Microstructures and enhanced mechanical properties of (Al3Ti+Al2O3)/Al–Si composites with co-continuous network structure prepared by pressure infiltration

The (Al₃Ti + Al₂O₃)/Al–Si composites with three-dimensional co-continuous network structures are fabricated by a pore-forming agent and the pressure infiltration technique. The effect of the Al₃Ti content on the mechanical and wear properties of the developed composites is investigated. The Al₂O₃ (alumina) formation, fracture, and wear mechanisms of the composites are also analyzed. The results demonstrate that the granular Al₂O₃ particles scatter around Al₃Ti phases which are synthesized in-situ during the sintering process. The 20 vol.% (Al₃Ti + Al₂O₃)/Al–Si composites possess the optimal mechanical properties, i.e., compressive and flexural strength of 585 MPa and 489 MPa, respectively, which are 64.8% and 46.0% higher than those of the matrix. The specific wear rate of the composites (16.5 × 10^?14 m³/Nm) is 79% lower than that of the matrix. By further increasing the Al₃Ti content, the network structure is completed, the wear resistance properties are improved, while the mechanical properties are decreased. The enhanced mechanical properties can primarily be attributed to the three-dimensional co-continuous network structure of the Al₃Ti and Al₂O₃ phases, as well as the pinning effect of Al₂O₃ particles.     

Preparation and mechanical performance of ductile Csf/Al2O3–BN composites—Part 2: Effects of fiber contents and ablation properties

In this paper, ductile C_sf/Al₂O₃–BN composites were prepared by hot-press sintering. Effects of fiber contents on the mechanical performance and ablation behavior of the composites were investigated systematically. The results showed that all the composites fractured in non-brittle failure mode, exhibiting elastic region and non-linear region as shown in load–displacement curves. With the increase in fiber contents from 15 to 30 vol%, mechanical properties of the obtained composites first increased, reached the peak values at fiber content of 25 vol% and then decreased. When being exposed to high-speed oxyacetylene combustion flow for 60 s, the composites with fiber contents of 15, 20 and 25 vol% showed comparable ablation property and mass loss of 5.3, 7.2 and 8.4×10⁻⁴ g/s, respectively. The ablation mechanisms include fiber and ceramic matrix oxidation, decomposition of mullite, evaporation of both B₂O₃ and SiO₂, and mechanical exfoliation.     

Preparation and characterization of Al2O3–25 mol% ZrO2 composites

Al₂O₃–ZrO₂ (AZ_x), with 25 mol% ZrO₂ content, was prepared using the co-precipitation method. Synthesized powders were characterized by thermal reaction using a differential thermal analysis technique (TG–DTA) and were investigated by phase formation using X-ray diffraction. It indicated that the reaction occurred at 850 °C; cubic (c)-ZrO₂ phase and Al₂O₃ were obtained. By increasing temperature to 1100 °C, tetragonal (t)-ZrO₂ phase was detected. The Al₂O₃–25 mol% ZrO₂ was sintered for 2 h in the temperature range of between 1300 and 1600 °C. The majority phases of ceramics were m-ZrO₂ and α-Al₂O₃, although a t-ZrO₂ phase also appeared as a minor phase and decreased with higher temperature. Moreover, morphology and particle size evolution have been determined via the SEM technique. SEM showed that the particles of powder are agglomerated and basically irregular in shape. An SEM micrograph of ceramics exhibits uniform microstructure without abnormal grain growth.     

Microstructure and phase transformation behavior of Al2O3–ZrO2 under microwave sintering

Zirconia is an inorganic, nonmetallic material with excellent properties. However, the brittleness of the zirconia, resulting from the thermal performance during the heating and cooling process, seriously limits the application of zirconia in the metallurgical, military, and aerospace industries. Al₂O₃ doped ZrO₂ was developed to improve the potential material's toughness. This paper studied the evolution of the surface functional groups, phase composition, toughening mechanism, and particle morphology of Al₂O₃ doped ZrO₂ during the heating process. Especially microwave heating was selected as the heating method during the experiments to save energy consumption. The results showed that the phase transition temperature was reduced by the microwave sintering technique, which also promoted the transformation between the m-ZrO₂ and t-ZrO₂, advancing the crystallinity and structural properties of the samples. The specific surface area shows a positive relationship with the microwave heating temperature, while the particle size of the powder decreased with the temperature increase. The optimized sintering effect appears at 1000 °C in the studied roasting temperature range (800 °C–1200 °C) for Al₂O₃–ZrO₂ powders. With the optimized sintering temperature, the void of the granular zirconia material was controlled, and the best micromorphology was obtained. In practical production, the application of microwave sintering and alumina doping is beneficial to saving costs and protecting the environment.