EBSD- and CT-analyses for phase evolution and crack investigations of thermal shocked flame sprayed alumina and alumina-rich structures

Due to the combination of lamellar structures composed of splats with special Al₂O₃-TiO₂-ZrO₂-compositions free-standing flame spraying coatings with a unique structure were produced. Because of thermal shock treatment, phase and crack evolution takes place. With the aid of EBSD- and CT-method the lamellar structure, the phase transition and the crack evolution were investigated and the prospect of these methods evaluated.     

Enhanced dielectric breakdown strength in Ni2O3 modified Al2O3-SiO2-TiO2 based dielectric ceramics

Dielectric ceramics have raised particular interest since they enable pulsed-power systems to achieve high voltage gradient and compact miniaturization. In this work, x wt%Ni₂O₃ doped Al₂O₃-SiO₂-TiO₂ based dielectric ceramics were prepared using conventional solid-state reaction and the effects of Ni₂O₃ on the crystal structure, dielectric properties and dielectric breakdown strength were investigated. It was found that with the doping of Ni₂O₃, the Al₂O₃-SiO₂-TiO₂ based dielectric ceramics became denser and the distribution of each phase was more uniform. For the composition of x?=?2.0, the dielectric breakdown strength was increased into 82.1?kV/mm, more than twice compared with that of the undoped one. In addition, the relationship between the dielectric breakdown strength and the resistance of Al₂O₃-SiO₂-TiO₂ based dielectric ceramics was discussed. The results show that the doping of Ni₂O₃ is a very feasible way to improve the dielectric breakdown strength and optimize the dielectric properties for the Al₂O₃-SiO₂-TiO₂ based dielectric ceramics.     

Sintering behavior,microstructural evolution,and mechanical properties of ultra-fine grained alumina synthesized via in-situ spark plasma sintering

Ultra-fine grained Al₂O₃ was fabricated by in-situ spark plasma sintering (SPS) process directly from amorphous powders. During in-situ sintering, phase transformation from amorphous to stable α-phase was completed by 1100 °C. High relative density over 99% of in-situ sintered Al₂O₃ was obtained in the sintering condition of 1400 °C under 65 MPa pressure without holding time. The grain size of in-situ sintered Al₂O₃ body was much finer (~400 nm) than that of Al₂O₃ sintered from the crystalline α-Al₂O₃ powders. For in-situ sintered Al₂O₃ from amorphous powders, we observed a characteristic microstructural feature of highly elongated grains in the ultra-fine grained matrix due to abnormal grain growth. Moreover, the properties of abnormally grown grains were controllable. Fracture toughness of in-situ sintered Al₂O₃ with the elongated grains was significantly enhanced due to the self-reinforcing effect via the crack deflection and bridging phenomena.     

Thermal aging of ceramics based on Al2O3-TiO2, Al2O3-SiO2 compositions

Conclusions Following an investigation of the thermal aging at 800°C in air of ceramics based on Al₂O₃ TiO₂ (Nos. 1–3) and Al₂O₃-TiO₂-SiO₂ (No. 4), it was established that the ceramics based on Al₂O₃-TiO₂-SiO₂ are the most heat-stable at 800°C over prolonged periods.Translated from Ogneupory, No. 1, pp. 21–23, January, 1990.     

Thermomechanical properties of ceramics in the systems Al2O3-TiO2 and Al2O3-TiO2-mullite

Conclusions We studied certain properties of ceramics in the systems Al₂O₃-TiO₂ and Al₂O₃-TiO₂-mullite, obtained by the use of the double-stage synthesis of aluminum titanate.We established the nature of the change in the high-temperature strength in relation to the ratio of Al₂O₃ and aluminum titanate. The maximum high-temperature strength (bending) at 1200°C is possessed by ceramic with a corundum matrix and a volume proportion of aluminum titanate equal to 40–45%.It is established that the addition of CaO + SiO₂ made in amounts of up to 1.0–1.5% contributes to the partial breakdown of the aluminum titanate in the compositions Al₂O₃-TiO₂ and the production of a ceramic with a bending strength of 160–190 N/mm² at 20–200°C, thermal-shock resistance 650–800°C, and thermal conductivity of 1.9–2.1 W/(m·K).We studied the effect of the mullite concentration on the properties of the ceramic in the system Al₂O₃-TiO₂-mullite. The introduction of mullite in amounts of not more than 50%, containing up to 3% of impurities, contributes to an increase in the ceramic's strength in the range 20–1300°C and in the thermal shock resistance.Translated from Ogneupory No. 2, pp. 22–26, February, 1988.     

Ultra-flexible Al2O3 fibers: A novel catalyst support material for sustainable catalysis

Flexible aluminum oxide (Al₂O₃) fibers were prepared by the blow spinning method and their potential as a high-temperature catalyst support was investigated. The synthesized Al₂O₃ fibers exhibited remarkable flexibility in both mechanical compression and recovery tests, which remained intact in a wide temperature range from −196 °C to 1200 °C. Moreover, their low thermal conductivity of 0.030 W K⁻¹∙m⁻¹, demonstrated an outstanding thermal insulation. Subsequently, nickel nanoparticles were uniformly distributed on the surface of the Al₂O₃ fibers as a self-supporting catalyst using a conventional impregnation method. The resulting self-supporting Ni/Al₂O₃ catalyst demonstrated remarkable thermo-catalytic performance and re-activation capability at high temperatures for thermocatalytic reaction of dry reforming of methane (DRM). Our findings highlight the potential of pure Al₂O₃ flexible fibers as a versatile material for various industrial applications, including high-temperature catalysis.     

Mechanism of in-situ formation of spinel and its effect on the mechanical properties of Al2O3–C refractories

This work looked at the in-situ formation mechanism of magnesia alumina spinel in Al₂O₃–C refractories with magnesia addition at different firing temperatures. A comprehensive study on the mechanical properties of Al₂O₃–C refractories was performed in comparison to traditional analogs. The magnesia alumina spinel was in-situ formed at the firing temperature of 1150 °C in Al₂O₃–C refractories. With the increase of the firing temperature, the Al₂O₃ phase was gradually dissolved in spinel phase to form aluminum rich spinel phase, resulting in a decrease in its lattice constant due to the defects formation. The formed spinel phase was homogenously distributed and bonded well with corundum, improving the interfacial bond, load transferring capacity and crack propagation resistance. The formation of spinel phase also enhanced the sintering of the alumina matrix owing to the solid solution of alumina in the spinel. Therefore, the mechanical properties such as cold modulus of rupture and hot modulus of rupture in Al₂O₃–C refractories achieved a substantial enhancement compared with traditional refractories.     

Dielectric strength of Al2O3/silicone composites after high‐temperature aging

Silicones are widely used for electrical insulation owing to their high dielectric strength and thermal stability. However, recent studies revealed insufficient stability of silicone for high‐temperature applications. To study the effect of Al₂O₃ fiber on silicone stability, we measured the dielectric strength of unfilled silicone and Al₂O₃/silicone composites as a function of aging time at 250°C in air and analyzed data by Weibull probability distribution to determine characteristic dielectric strength (E₀) and shape parameter (β). Prior to aging, unfilled silicone and composites had similar behavior, with E₀ at about 20 kV/mm and β > 15. During aging, unfilled silicone developed both micro‐ and macrocracks, with β dropped below five in 240 h and E₀ decreased significantly. Composites developed microcracks, with β dropped below 5 in longer time and E₀ remained almost constant. Addition of Al₂O₃ slowed down crack growth in silicone matrix, resulting in longer lasting high‐temperature dielectric materials. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2014 , 131, 41170.     

High damage tolerant Al2O3 composite ceramics constructed with short Al2O3 fibers

The catastrophic fracture characteristics of ceramic materials have become one of the most serious factors limiting their application in critical areas, as a result, it is urgent to overcome the brittleness and improve the damage tolerance of ceramic materials. Herein, a series of Al₂O₃ composite ceramics developed with short Al₂O₃ fibers and a compound interface phase composed of Al₂O₃ and h-BN powders, followed by investigating their fracture behaviors and damage tolerance. Results show that these composites present progressive fracture manners with the rising resistance curve (R-curve) behaviors, and the maximum crack growth toughness of the sample with 15% compound interface phase reaches above 10 MPa·m^1/2 (135% increase with respect to the reference alumina). Meanwhile, the composite ceramic exhibits an excellent ability to resist catastrophic failure with a large critical crack size (105.47 ± 19.11 μm) and high damage tolerance parameter (0.71 ± 0.06 m^1/2), which are close to 14.57 times and 5.92 times higher than those of the reference alumina. The superior performances are mainly attributed to the precise combination of compound interface phase for inducing crack and interlocking Al₂O₃ fibers for load capacity.     

Fracture toughness determination of Ti3Si(Al)C2 and Al2O3 using a single gradient notched beam (SGNB) method

In this work, we suggest a new and simple method named single gradient notched beam (SGNB) method for determining the fracture toughness of Ti₃Si(Al)C₂ and Al₂O₃ with four-point bending specimens. For the specimen with a gradient notch, a sharp natural crack will initiate and extends from the tip of the triangle under increasing load. Based on the straight through crack assumption or on the slice model, the stress intensity factor coefficient for this notched beam was derived. The fracture toughness can be calculated from the maximum load and the minimum of the stress intensity factor coefficient without knowing the crack length. To verify the feasibility and reliability of this suggested method, the SGNB method and two other conventional methods, e.g. the chevron notched beam (CNB) method and single edge notched beam (SENB) method, were performed to determine the fracture toughness of Ti₃Si(Al)C₂ and Al₂O₃. The measured fracture toughness values obtained from the SGNB method agreed well with those from conventional fracture toughness tests.     

Impact of Al2O3-40 wt.% TiO2 feedstock powder characteristics on the sprayability,microstructure and mechanical properties of plasma sprayed coatings

Atmospheric plasma sprayed (APS) Al₂O₃-TiO₂ coatings have found a wide range of industrial application due to their favorable properties, combined with low costs and a high availability. However, the detailed effect of the phase composition and the element distribution of the feedstock powders on the coating properties and the spraying process have only crudely been investigated so far. Here the impact of aluminum titanate (Al₂TiO₅) on the microstructural features and mechanical properties of Al₂O₃-40 wt.% TiO₂ APS coatings is demonstrated by investigating the detailed phase composition and the distribution of aluminum and titanium in three fused and crushed feedstock powders and the respective coatings. Thereby, a direct influence of Al₂TiO₅ content on the deposition efficiency, the porosity, the elastic modulus, and the hardness of the coatings is revealed. The results emphasize the need for a more detailed specification of commercial Al₂O₃-TiO₂ feedstock powders to ensure a high reliability of the coating properties.     

Fatigue Crack Growth Behavior of Silicon Nitride: Roles of Grain Aspect Ratio and Intergranular Film Composition

The role of microstructure in affecting the fatigue crack growth resistance of grain bridging silicon nitride ceramics doped with rare earth (RE = Y, La, Lu) oxide sintering additives was investigated. Three silicon nitride ceramics were prepared using MgO‐RE₂O₃ and results were compared with a commercial Al₂O₃‐Y₂O₃‐doped material. Decreasing stress intensity range (ΔK) fatigue tests were conducted using compact‐tension specimens to measure steady‐state fatigue crack growth rates. Specimens doped with MgO‐RE₂O₃ additives showed a significantly higher resistance to crack growth than those with Al₂O₃‐Y₂O₃ additives and this difference was attributed to the much higher grain aspect ratio for the MgO‐RE₂O₃‐doped ceramics. When the crack growth data were normalized with respect to the total contribution of toughening by bridging determined from the monotonically loaded R‐curves, the differences in fatigue resistance were greatly reduced with the data overlapping considerably. Finally, all of the MgO‐RE₂O₃‐doped silicon nitrides displayed similar steady‐state fatigue crack growth behavior suggesting that they are relatively insensitive to the intergranular film.     

Fracture behavior of Al2O3–SiO2 castables by the wedge splitting test and digital image correlation technique

The fracture mechanisms are helpful for the optimization and design of toughness and microstructure of refractories. Fracture behavior of ultra-low cement bonded Al₂O₃–SiO₂ castables was researched using the wedge splitting test coupled with digital image correlation technique (WST-DIC). Flexibility of Al₂O₃–SiO₂ castables is improved by introducing andalusite aggregates into the castables. The characteristic length L_CH, a parameter used to assess flexiblity of materials, was observed to reach 287.2 mm in andalusite-containing Al₂O₃–SiO₂ castables, more than 5 times that of reference castables. Microcracks toughening is the main toughening mechanisms for flexibility improvement of the Al₂O₃–SiO₂ castables containing andalusite. Microcrack network in the Al₂O₃–SiO₂ castables could be designed by exploiting the volume expansion caused by mullitization of andalusite and the coefficient of thermal expansion (CTE) mismatch between the andalusite aggregate and the matrix. Unlike andalusite-free castables, castables containing andalusite possess a distinct fracture process zone (FPZ), the crack branching and deflection can be observed around the main crack during the fracture process, which leads to the prolong of the crack propagation path, the increase of the dissipation energy during the fracture, and the enhancement of resistance to crack propagation.     

Grain growth kinetics in microwave sintered graphene platelets reinforced ZrO2/Al2O3 composites

The grain growth kinetics and mechanical properties of graphene platelets(GPLs) reinforced ZrO₂/Al₂O₃(ZTA) composites prepared by microwave sintering were investigated. The calculated grain growth kinetics exponent n indicated that the GPLs could accelerate the process of the Al₂O₃ columnar crystal growth. And the grain growth activation energy of the Al₂O₃ columnar crystal indicated that the grain growth activation energy of the GPLs doped ZTA composites is much higher than those of pure Al₂O₃ and ZTA in microwave sintering. The optimal mechanical properties were achieved with 0.4?vol% GPLs, whose relative density, Vickers hardness and fracture toughness were 98.76%, 18.10?GPa and 8.86?MPa?m^1/2, respectively. The toughening mechanisms were crack deflection, bridging, branching and pull-out of GPLs. The results suggested that GPLs-doped are good for the Al₂O₃ columnar crystal growth in the ZTA ceramic and have a potentially improvement for the fracture toughness of the ceramics.     

Improved Crack Healing and High‐Temperature Oxidation Resistance of Ni/Al2O3 by Y or Si Doping

Recovery of mechanical strength was investigated for 5 vol% Ni/α‐Al₂O₃ nanocomposites that had improved resistance to high‐temperature oxidation by doping with Y or Si (Ni/Al₂O₃‐Y and Ni/Al₂O₃‐Si). Surface cracks disappeared completely because of the oxidation product, NiAl₂O₄. The fraction of crack disappearance was comparable between Ni/Al₂O₃‐Y and Ni/Al₂O₃‐Si. The apparent activation energy of crack healing is similar to the grain‐boundary diffusion of Ni ions in an Al₂O₃ matrix. The rate‐controlling process of crack healing is the grain‐boundary diffusion of cations in an internally oxidized zone (IOZ) of the Ni/Al₂O₃ system. The bending strengths of the as‐sintered and as‐cracked Ni/Al₂O₃‐Y samples were 561 and 232 MPa, respectively. Heat treatment at 1200°C for 6 h resulted in a recovery of the bending strength up to 662 MPa for Ni/Al₂O₃‐Y as well as 606 MPa for Ni/Al₂O₃‐Si. Y and Si dopants were segregated into the Al site at the Al₂O₃ grain boundaries, and then, enhanced covalent bonding occurred with neighboring oxygen. While the flux of Ni ions was retarded slightly by doping with Y and Si, a shorter IOZ provided enough Ni ions to form NiAl₂O₄ on the surface. Ni/Al₂O₃‐Y and Ni/Al₂O₃‐Si have the desirable properties of crack healing and resistance to high‐temperature oxidation.     

Influence of carbonaceous materials on the interactions among (Al2O3-C)/Fe system with temperature and soaking time

It has practical significance for improving the service life of Al₂O₃-C refractories and reducing its influence on steel quality to reveal the reaction mechanism among (Al₂O₃-C)/Fe system under high temperature. The influence of carbonaceous materials on the interactions among (Al₂O₃-C)/Fe system with temperature and soaking time were studied using thermalgravity method in this paper in order to get a better understanding on the reaction mechanism among (Al₂O₃-C)/Fe system. The weight loss of (Al₂O₃-C)/Fe samples and the formation of Al₂O₃ crystal whiskers along with the change of aluminium and carbon content in iron indicates the mechanism of the effects of carbonaceous materials on the reactions among (Al₂O₃-C)/Fe system under high temperature. The result showed that the aluminium pickup of iron was not only due to the dissolution of Al₂O₃ in molten iron but mostly due to the carbothermic reduction of Al₂O₃ and carbonaceous materials in the presence of molten iron.     

Influence of metallic properties on the fracture characteristics of Al2O3/Ti/Ni-laminated composites

The mutual confinement of ceramics and metals in laminated composites tends to change the original properties of ceramics and metals. In this study, two kinds of laminated composites, Al₂O₃/Ti and Al₂O₃/Ti/Ni, were prepared. Three-point bending experiments revealed that Al₂O₃/Ti underwent brittle fracture after elastic deformation. The fracture morphology analysis revealed that the Ti in Al₂O₃/Ti became brittle due to the formation of columnar crystals. The temperature gradient perpendicular to the direction of laminations during preparation was responsible for the formation of columnar crystals. The force–displacement curves of the Al₂O₃/Ti/Ni combine the properties of elastic deformation of ceramics and plastic deformation of metals. The reason why the Al₂O₃/Ti/Ni did not fracture completely in the bending experiments is that Ni maintained the toughness, and there is a good interfacial bond among Al₂O₃, Ti, and Ni. The indentation crack analysis revealed that cracks have long transverse propagation and short longitudinal propagation in both laminated composites. Finite element analysis revealed that this was due to compressive stress in the Al₂O₃ layer and tensile stress in the metal layer. This compressive stress consumes the crack energy in the longitudinal direction and stops the crack in the metal layer. The brittle to ductile gradient transition among Al₂O₃, Ti, and Ni, combined with the guidance of crack propagation direction by the interfacial layer, enhances the ability of Al₂O₃/Ti/Ni to resist damage.     

Preparation and characterization of Cr2O3-TiO2-Al2O3-V2O5 green pigment

Green pigments with high near infrared reflectance based on a Cr₂O₃-TiO₂-Al₂O₃-V₂O₅ composition have been synthesized. Cr₂O₃ was used as the host component and mixtures of TiO₂, Al₂O₃ and V₂O₅ were used as the guest components. TiO₂, Al₂O₃, and V₂O₅ were mixed into 39 different compositions. The spectral reflectance and the distribution of pigment powder were determined using a spectrophotometer and a scanning electron microscope, respectively. It was found that a pigment powder sample S9 with a Cr₂O₃-TiO₂-Al₂O₃-V₂O₅ composition of 80, 4, 14 and 2 wt%, respectively, gives a maximum near infrared solar reflectance of 82.8% compared with 49.0% for pure Cr₂O₃. The dispersion of pigment powders in a ceramic glaze was also studied. The results show that the pigment powder sample S9 is suitable for use as a coating material for ceramic-based roofs.     

Composite wear-resistant glass ceramic materials with various fillers

A comparative analysis of the physicomechanical properties of composites based on sitallizable glass of the CaO-BaO-Al₂O₃-TiO₂-SiO₂ system with different fillers (Al₂O₃, ZrO₂, and CrO₃ industrial oxides) was performed. It was established that the best filler is Al₂O₃. However, ZrO₂ and Cr₂O₃ fillers also improve the mechanical properties of the composites rather substantially.Translated from Steklo i Keramika, No. 3, pp. 14–15, March, 1995.     

Development of input output relationships for self-healing Al2O3/SiC ceramic composites with Y2O3 additive using design of experiments

Al₂O₃/SiC ceramic composites with Y₂O₃ as an additive, was synthesized using the Taguchi method of design of experiments, so as to develop statistically sound input output relationships. The proportion of SiC was varied from 12 to 21 vol.% whereas that of Y₂O₃ was varied from 2.5 to 4 vol.%. The composites were sintered at 1500 °C for a soaking time period of 12 h in an air atmosphere. Cracks were induced on the composite surface using a Vickers indenter with a load varying between 20 and 40 kg. Fractographical analyses have been carried out using optical and/or scanning electron microscopy to investigate the surface crack propagation behavior. Thermal aging at 1300 °C in the time range of 0.5-12.5 h was applied to find optimal conditions for healing of the pre-cracked samples. The output parameters such as crack length, healed crack length, hardness and fracture toughness of the samples were correlated with appropriate inputs such as contents of SiC and Y₂O₃, crack-healing temperature, healing time, compaction pressure, indentation load using statistical analysis. Further, the extent of influence, exerted by pertinent input parameters on output parameters, was also identified.