Silica-based ceramic core for aviation applications: Facile pore filling and flexural strength improvement

The effect of alumina addition on the pore filling process, crystallization behavior and mechanical properties of silica-based ceramic cores was investigated. The sintered samples at 1250°C were treated at 1550°C for 0.5 hour in order to simulate a casting process condition. The microstructure analysis indicated that an appropriate alumina addition enhanced the pore filling process by supplying a substantial liquid viscous flow. With an increase in the liquid viscous flow, smaller pores were filled first, and larger pores were filled later. The results also indicated that the pore filling process could be enhanced by adding small powder additives to decrease the pore size between the particles in the ceramic material. However, an excessive alumina addition in the silica-based ceramic cores had a negative effect on the flexural strength and leaching rate. As the alumina content increased from 8 to 12 wt%, the flexural strength of the ceramic core decreased from 16.37 to 4.60 MPa, respectively, and the leaching rate also decreased obviously. These results were explained by an acceleration in crystallization trend of the fused silica particle surface and the merging of connected pores in the sintered body.     

Enhanced thermal properties of silica-based ceramic cores prepared by coating alumina/mullite on the surface of fused silica powders

In this study, an alumina/mullite coating was synthesized on the surface of fused silica powders to form an alumina/mullite-silica core-shell structure. The effects of the alumina/mullite coating on the cristobalite crystallization, thermal properties, and leachability of the silica-based ceramic cores were investigated using the simulated casting process. The X-ray diffraction results indicated that the crystallization of cristobalite was significant at the simulated casting temperature of approximately 1400 °C. An increase in the cristobalite content during this stage resulted in a large thermal expansion because of its higher coefficient of thermal expansion compared with that for fused silica. The addition of optimum amounts of the alumina/mullite powders resulted in an increase in the initial shrinkage temperature and a decrease in the shrinkage of the specimens. When the coating powders were added at 43 wt%, the initial shrinkage temperature increased from 1092 °C to 1200 °C and the shrinkage decreased sharply. Leaching tests showed that the silica-based ceramic cores were removed in the form of stripped layers. The washing and shaking process accelerated the disintegration of the ceramic core and improved its leachability.     

Effect of fine alumina in improving refractoriness of ceramic shell moulds used for aeronautical grade Ni-base superalloy castings

This paper discusses an improvement in shell refractoriness and dimensional stability of columnar grained (CG) low pressure turbine blade castings made using Ni base superalloy by directional solidification process (DS). Two ceramic shell systems were adopted, namely shell system I and II. Shell moulds were prepared by using ceramic slurries containing zircon flour as a filler material and colloidal silica as a binder. As compared to shell system II (zircon filler with colloidal silica binder and fine alumina), shell system I (zircon filler with colloidal silica binder) showed lower refractoriness. Shell system II showed an increase in the flexural strength both in the green as well as in fired conditions. Shells made from shell system II showed about 13% higher green strength and 55% higher fired strength as compared to shell system I. Shell system II also exhibited superior self sag resistance up to 1625?°C. Moulds prepared from this shell system yielded aeronautical grade casting with high dimensional accuracy even at a metal pouring temperature of 1550?°C. Moulds from shell system I, on the other hand, underwent sagging even at metal pouring temperature of 1500?°C, leading to dimensionally unacceptable castings. The superior performance of shells prepared from shell system II can be ascribed to the presence of fine alumina in the shell.     

Properties of alumina coatings prepared on silica-based ceramic substrate by plasma spraying and sol-gel dipping methods

Silica-based ceramic cores are widely used in the manufacturing of hollow, nickel-based, superalloy turbine blades. However, elemental Hf, Ti, Al, and other active metals in the superalloy can react with silica-based ceramic cores during casting, resulting in a reduction in the quality of the turbine blades. In this study, both plasma spraying and sol-gel dipping methods were used to prepare alumina coatings on silica-based ceramic substrates to prevent the interfacial reaction. The performance of the alumina coatings prepared by both methods was evaluated by comparative analysis of the surface roughness, bonding interface morphologies, and the adhesive characteristics of the coating. The plasma-sprayed alumina coating has a roughness greater than 5 μm and peeled away from the substrate due to the difference in thermal expansion between SiO₂ and Al₂O₃ at temperatures above 1500 °C, rendering the silica-based substrate with the plasma-sprayed alumina coating unfit for the application requirements of the casting process. The alumina coating prepared by the sol-gel dipping method improved the roughness of the substrate from Ra 2.39 μm to Ra 1.83 μm, and no peeling was observed when heated to 1550 °C for 30 min due to the pinning characteristics of the coating on the substrate. Furthermore, the interfacial reaction between the DZ125 superalloy melt and the silica-based substrate coated with alumina by sol-gel dipping method were investigated. The alumina coating effectively inhibited the interfacial reaction and no reaction products were detected during the directional solidification with pouring temperature of 1550 °C and withdraw rate of 5 mm/min. While a uniform, 4–5 μm thick HfO₂ reaction layer formed between the uncoated substrate and the DZ125 alloy melt. Two dipping-drying cycles were required to ensure the alumina sol completely covered the surface of the substrate.     

Improved collapse properties of silica-based ceramic cores via flexibly regulating cristobalite content

Although silica-based ceramic cores have important applications in the precision casting of metallic devices, their high-temperature stability and removal performances are seriously affected by the liquid phase sintered fused silica. Herein, we develop a manufacturing strategy of high-collapse silica-based ceramic core via using cristobalite crystals as the sintering inhibitor, waterglass as the binder, and injection moulding at 100°C and 80 MPa, followed by heat treatment simulating the casting process for sintering at 1200°C and 1500°C. The results demonstrated that the addition of cristobalite crystals could effectively form the core skeleton to ensure high-temperature performance. Meanwhile, it inhibited the liquid flow during sintering and induced the crytsallization from fused SiO₂ glass into cristobalite crystals, and the resulting plenty of micropores and microcracks within the microstructure effectively improve the removal performance. Especially, the porosity was highest up to 35.36% and the flexural strength was only 6.74 MPa when the addition of cristobalite reached 45%, realizing a 100% removing by high-frequency and fast-speed specific mechanical vibration. And, the casting is guaranteed to be flat and free of defects. This work provides a simple and flexible strategy to manufacture high-collapse silica-based ceramic cores, which can be removed by specific mechanical vibration without immersion in acid or alkali solutions after casting.     

Anisotropy management on microstructure and mechanical property in 3D printing of silica-based ceramic cores

Ceramic core is an essential component in the precise casting of hollow turbine blades, and the investigation on 3D printing of silica-based ceramic cores is crucial to the development of aviation industry; however, they are suffered from difficulty in high-temperature strength and structural anisotropy. In present work, silica-based ceramic cores were prepared via DLP stereolithography 3D printing, and the anisotropy management on microstructures and properties were explored based on the particle size of fused silica powders. In 3D printed ceramic cores with coarse powders, significant anisotropy was displayed exhibiting multilayer structure with large gaps in horizontal printing and uniform porous microstructure in the vertical direction, which was further explained by the particle deposition in printing. With finer silica powders, the uniformity in the microstructures was highly improved, attributed to the enhanced particle dispersion in ceramic slurries and promoted interlayer particle rearrangement during sintering. To evaluate the anisotropy in mechanical property, the ratio of vertical strength to horizontal strength (σ_V/σ_H) was proposed, which rose from 0.48 to 0.86 as the particle size decreased from 35 µm to 5 µm, suggesting enhanced mechanical uniformity. While the average particle size of silica powders was 5 µm, the flexure strengths of ceramic cores in different directions were up to 18.5 MPa and 16.3 MPa at 1540 °C with σ_V/σ_H ratio of 0.88, which well satisfied the demands for the casting of turbine blades. This work inspires new guidance on the anisotropy management in ceramic cores prepared by 3D printing, and provides new technology for fabrication of silica-based ceramic cores with superior high temperature mechanical properties.     

Investigation on cristobalite crystallization in silica-based ceramic cores for investment casting

In this work, cristobalite crystallization and its effects on mechanical and chemical behaviour of injection moulded silica-based ceramic cores were investigated. In order to simulate casting process condition, the sintered samples at 1220 °C were also heated up to 1430 °C. Flexural strength test was carried out on both sintered and heat treated samples. Chemical resistance of the cores was evaluated by leaching the samples inside 43 wt% KOH solution at its boiling point. Phase evolution and microstructure were investigated by thermal analyses (DTA and DSC), X-ray diffraction (XRD), scanning electron microscopy (SEM) and optical microscopy (OM). Results showed that cristobalite was crystallized on the surface of fused silica grains at about 1380 °C. Flexural strength of the sintered cores was decreased after simulated casting heat treatment due to cristobalite phase transformation. The formed cristobalite on the surface of fused silica grains dramatically decreased the leachability of ceramic cores.     

Alumina-zircon filler based ceramic shell moulds for directionally solidified cast shrouded low pressure turbine blades

Ceramic shell moulds for investment casting of shrouded low-pressure turbine (LPT) blades were prepared by using colloidal silica binder and partial substitution of the zircon filler with fine alumina. Among the two ceramic slurry systems designed, the first slurry system comprised of polymer-free colloidal silica binder, and the second slurry system comprised of polymer-containing colloidal silica binder. The samples prepared from the first slurry system showed higher fired residual strength and self-load sag values (lesser sag resistance). The casting of shrouded LPT blades was carried out at 1525 °C and 1550 °C using CM247LC superalloy. Ceramic shell moulds prepared from the second slurry system, containing 30 wt% of fine alumina filler, yielded aeronautical grade casting (at 1550 °C) of blades with required dimensional accuracy and average surface roughness. Microstructural analysis of the cut surfaces of self-load sag tested samples was carried out to understand the effect of fine alumina substitution on shell characteristics.     

High strength silica-based ceramics material for investment casting applications: Effects of adding nanosized alumina coatings

A nanosized alumina coating was synthesized on the surface of fused silica particles by electrostatic attraction. The effects of the coated fused silica particles on the cristobalite crystallization behavior, microstructure evolution, and flexural strength of silica-based ceramic cores were investigated. X-ray diffraction (XRD) was used to characterize phase transformations in the specimens, and the results indicated that the formed nanosized alumina coatings could retard cristobalite formation by inducing compressive stress on the fused silica particle surface. A mullite phase was also found due to the reaction of the nanosized alumina coating and the surface of the fused silica when the sintering temperature was increased to 1300 °C. Analysis using scanning electron microscopy equipped with energy dispersive spectrometry (SEM/EDS) suggested that alumina nanoparticles in the coated layer dispersed into a liquid phase and formed a barrier layer to impede the movement of the liquid phase, preventing the pore-filling process and increasing the open porosity of the ceramic specimens. Flexural strengths at room temperature were tested, indicating that increases in the sintering temperature of the specimens without coated fused silica powders had little effect on flexural strength. However, the flexural strength of the specimens with coated fused silica powders increased with increases in sintering temperature. The improvement in flexural strength was related to the reinforcement by sintering necks between particles and the improvement in the strength of the coated fused silica powder.     

Advanced ceramics from a preceramic polymer and nano-fillers

A commercial silicone resin (“silicone”) filled with ceramic nanoparticles has been employed for the preparation of mullite and β-SiAlON ceramics. Dense, pure, crack free mullite were prepared by the heating in air of a mixture of silicone resin and alumina nanoparticles in the temperature range 1200–1550 °C. The high reactivity of Al₂O₃ towards silica, coupled with nanometric size, led to a large volume fraction of mullite crystals even at low firing temperatures (1250 °C). β-SiAlON ceramics were prepared by the heating of a mixture of silicone resin and fillers consisting of Al₂O₃ nanoparticles and Si₃N₄ and AlN microparticles, in the temperature range 1450–1550 °C in nitrogen atmosphere. The formation of SiAlON was found to be preceded by the formation of intermediate alumino-silicate phases like mullite and sillimanite, successively reduced (due to the carbon content of the ceramic residue of silicone resins) and nitrided. Although some oxide contamination was still present after the high temperature treatment, a high β-SiAlON yield (about 80%) was achieved. The use of nano-filled silicones provides a promising route for the fabrication of advanced ceramic components by exploiting polymer processing techniques, with the achievement of complex shapes.     

SiAlON ceramics from preceramic polymers and nano-sized fillers: Application in ceramic joining

Commercial polysiloxanes filled with alumina nano-particles have been employed for the preparation of β-SiAlON-based ceramics in the temperature range 1450–1550 °C in nitrogen atmosphere. The formation of β-SiAlON was found to be preceded by the formation of intermediate alumino-silicate phases. The SiAlON yield was affected by the occurrence of phase separation in the oxycarbide ceramic residue (SiOC) derived from the silicones and by the partial vaporization of silica, by reduction into gaseous SiO, leading to products with an oxide contamination, consisting of corundum. Filled silicones finally found a promising application in the ceramic joining, sandwiched between two pre-existing α–β (Yb-)SiAlON pieces and treated at high temperature (1550 °C): with a proper formulation, a significant inter-diffusion was observed between the joining layer and the SiAlON parts, causing the evolution of a homogeneous joint region, matching the microstructure and the mechanical properties of the parent ceramics. The pre-oxidation of the SiAlON, generally aiding the wetting of the joining media prior to thermal treatment, showed no significant benefit on the microstructure. On the contrary, the addition of a small load during the thermal treatment allowed the formation of strong joints, not exhibiting any significant difference in mechanical properties with the parent material.     

Microstructure and properties of high alumina castables containing calcium alumino‐titanate

Calcium alumino‐titanate (CAT)‐containing high alumina castables were prepared using bauxite, CAT, and α‐Al₂O₃ as starting materials, and subsequently heat treated at various temperatures ranging from 1400°C to 1600°C. The thermo‐mechanical properties of the specimens as a function of the temperature were characterized in terms of linear shrinkage, bulk density, apparent porosity, cold crushing strength (CCS), modulus of rupture (MOR), residual ratio of MOR, and coefficient of thermal expansion (CTE). X‐ray diffraction (XRD) and scanning electron microscopy (SEM) were used to determine the phase composition and microstructural evolution, respectively. Sintering at temperatures between 1450 and 1500°C promoted normal grain growth, with the formation of a granular surface contact, and abnormal grain growth occurred at higher temperatures (≥ 1550°C). The cold strength of the specimen initially increased and subsequently decreased with temperature, whereas the residual ratio of MOR initially decreased with increasing temperature to 1550°C, then increased above 1550°C. In addition, the CTE of the specimen was only minimally influenced by the firing temperature.     

Fabrication of transparent Y2O3 ceramics with record-high thermal shock resistance

Sintering-additive-free fine-grained highly transparent Y₂O₃ ceramics featuring record-high thermal shock resistance were fabricated using commercial powders via vacuum pre-sintering (1375–1550?°C) followed by hot-isostatic pressing (1450?°C). The sample pre-sintered at 1450?°C provides the optimum microstructure for post HIPing, which resulted in a grain size of 0.64?μm. The transmittance, microhardness and fracture toughness of the thus HIPed sample are 80.8% at 1100?nm and 65.5% at 400?nm (1.2?mm thick), 8.0?±?0.02?GPa and 1.00?±?0.06?MPa?m^1/2, respectively. The thermal conductivity increases from 13.1 to 16.5?W/m/K with increasing vacuum pre-sinterin Proc. SPIE-Int. Soc. Opt g temperature from 1450 to 1550?°C. This hybrid sintering method realized high thermal conductivity and high strength simultaneously. Consequently, the thermal shock resistance of the HIPed specimen vacuum pre-sintered at 1450?°C in this work is the highest ever reported to the best of our knowledge, which makes the developed material a promising candidate for high-power laser host and IR dome.     

Study on preformed and in situ spinel containing alumina castable for steel ladle: Effect of fume silica content

In the present study, the effect of fume silica content on preformed and in situ spinel containing alumina spinel castable was studied by varying fume silica content at 1 and 4 wt.%. Spinel content for preformed alumina spinel castables varied from 10 to 30 wt.% and MgO content for in situ alumina spinel castables varied from 2.8 to 8.4 wt.%, respectively, and the distribution coefficient (q value) was maintained at .21 and .29 as per Dinger and Funk model. Different castable compositions were processed as per conventional processing technique and further evaluated for densification and strength studies after heat treatment at 110, 1000, and 1550°C. Fired samples at 1550°C were further evaluated for the hot modulus of rupture study at 1400°C and phase analysis study of the matrix phase. Also, the fired samples were studied for microstructural evaluation.     

Influence of silicon carbide as a mineralizer on mechanical and thermal properties of silica-based ceramic cores

Ceramic cores have been designed with compounds based on fused silica due to its excellent thermal stability and chemical inertness against molten metals. To endure the high temperatures present during investment casting, mineralizers have been widely used to enhance the flexural strength and shrinkage of ceramic cores. In this study, we demonstrated a silica-based ceramic core with silicon carbide as a mineralizer for improving the mechanical and thermal properties. The SiC in the silica-based ceramic cores can enhance the mechanical properties (i.e., flexural strength and linear shrinkage) by playing a role as a seed for the crystallization of fused silica to cristobalite. The SiC also improves the thermal conductivity due to its higher value compared with fused silica. The results suggest that using the optimal amount of silicon carbide in silica-based ceramic cores can provide excellent mechanical properties of flexural strength and linear shrinkage and improved thermal conductivity.     

Evaluation of the morphology and pore characteristics of silica refractory using X-ray computed tomography

Silica refractory has excellent high-temperature performance, but its apparent porosity is relatively high. In this work, samples obtained before and after creep testing of silica brick (1550 °C, 50 h), from used silica checker brick (existing only tridymite and amorphous) and from used dome brick (existing only cristobalite and amorphous) were investigated using a three-dimensional structure model based on X-ray computed tomography (CT). The results show that the porosity of silica brick was high but consisted mainly of interconnected pores, with a very small proportion of closed pores (smaller after long-term use). During the use of silica brick, the morphology and phase transformation caused large particles to rupture, and the mineralizer became liquid at high temperature. The broken particles and interconnected pores provided channels for the migration of the liquid in the brick at high temperature. The silica brick presented a homogeneous ceramic structure during long-term operation. Tridymite or cristobalite presented a solid frame leading to an excellent creep performance of the silica brick (the creep rate of the checker brick was ?0.16% at 1550 °C for 50 h). Results were discussed, compared with literature and a model for the transformation of the silica brick from a refractory structure to a homogeneous ceramic structure was established in this paper.     

Microporous alumina substrate with porosity >70% by gelcasting

Microporous alumina membrane substrate in tubular and planar configurations have been prepared by gelcasting of alumina powder slurry using high amount of urea–formaldehyde as gelling agent followed by humidity controlled drying, binder removal and sintering of the gelled bodies. Porosity of the substrate samples sintered at 1350 °C was more than 70% as measured by mercury porosimeter. More than 51% porosity could be retained even after sintering of the samples at 1450 °C. Average pores size of the membrane substrate samples sintered at temperature in the range from 1250 to 1550 °C varied between 0.42 and 0.56 with a maximum at 1350 °C. More uniform pores were observed in sample sintered at 1450 °C. Urea-formaldehyde polymer present in the gelcast body acts as template for micropores.     

Controlled anisotropy in 3D printing of silica-based ceramic cores through oxidization reaction of aluminum powders

Ceramic cores are key components to form inner hollow structures in aero-engine blades, and 3D printing is an ideal molding technology for ceramic cores. In this work, silica-based ceramic cores are fabricate via 3D printing of digital light processing (DLP) stereolithography, and the anisotropy in microstructure and property are controlled by aluminum powders. The ceramic cores without aluminum powders exhibit anisotropic microstructure with interlayer gaps, which get narrower and disappear with doping of 7.5–10 wt% of aluminum powders, due to the volume expansion during oxidization reaction of aluminum powders filling the interlayer gaps. The anisotropy in mechanical property is rely on the printing direction, and the ratio of strength in different directions (σ_V/σ_H) is put forward to value the mechanical anisotropy; the ratios rise from 0.40 to 0.92 at room temperature and 0.51 to 0.97 at 1540 °C, as 7.5 wt% of aluminum is doped, and the optimized ceramic cores show high-temperature strengths of 16.6 MPa and 16.1 MPa in different printing directions. Even though ceramic cores with 10 wt% of aluminum show uniform microstructure and higher σ_V/σ_H ratio, the weak particle bonding within printing layers limits their mechanical property, and the strengths decrease to 13.8 MPa and 13.4 MPa at 1540 °C. This work inspires a new technique to excellent high-temperature mechanical properties with anisotropy control in 3D printing of ceramic cores.     

Effects of micro-sized mullite on cristobalite crystallization and properties of silica-based ceramic cores

Silica-based ceramic cores are extensively used in investment casting process, during which they must exhibit sufficient flexural strength and deformation resistance. In this study, micro-sized mullite was used as an additive to silica-based ceramic cores to optimize their high temperature properties. To investigate the effects of micro-sized mullite on cristobalite crystallization, mechanical and thermal properties of silica-based ceramic cores, ceramic cores with different amounts of micro-sized mullite were fabricated. The XRD results showed that additional micro-sized mullite diminished the crystallization of cristobalite at high temperatures, primarily caused by the mullite related compressive stresses on the surface regions of fused silica particles. Three-point bending tests and SEM results showed that micro-sized mullite had a more significant effect on the flexural strength of ceramic cores compared with conventional additives. Particularly, the fracture mechanism of silica-based ceramic cores had been changed from intergranular fracture into a mixed fracture consisting of both intergranular and transgranular fracture. The mechanical and thermal properties of ceramic cores were all reduced slightly as the mullite content exceed 4.6 wt%. Hence, to optimize the properties of silica-based ceramic cores, the micro-sized mullite content should not exceed 4.6 wt%.     

Additive manufacturing of low-shrinkage alumina cores for single-crystal nickel-based superalloy turbine blade casting

We prepare bimodal particle size photo-curable ceramic pastes with high solid loadings (up to 65 vol %) and fabricate porous alumina ceramic cores with complex shapes via ceramic stereolithography (Cer-SLA) 3D printing technique. The sintering temperature is carefully selected, ranging from 1500 °C to 1650 °C, and a high holding time (>4 h) is applied to guarantee that the materials can withstand the subsequent high temperature (>1500 °C) casting process for single-crystal nickel-based superalloy hollow turbine blades. Herein, the originally spherical fine particles are found to become platelet-like after sintering, and the forming mechanism is discussed in detail. In addition, we explore the influence of platelet-like particles, coarse particles and sintering process on the microstructural evolution of alumina particles, and reveal the relationship between microstructure and properties of ceramic cores. These results illustrate that the proposed materials for SLA 3D printing exhibit a great potential in the fabrication of complex-shaped alumina ceramic cores for high-precision investment casting, e.g., manufacturing single-crystal nickel-based superalloy hollow turbine blades for an advanced aircraft engine.