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.     

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.     

Investigation of microstructure evolution and properties in silica-based ceramic cores with alumina as a mineralizer

In this work, silica-based ceramic cores with alumina as a mineralizer were prepared via an injection molding method, and the effects of alumina on the microstructural evolution and properties at 1450°C (simulating the process of equiaxed castings) and 1550°C (simulating the process of columnar/single crystal castings) were investigated. It was found that alumina promoted the cristobalite crystallization of fused silica refractory during sintering but inhibited the devitrification rate in the subsequent heating. The flexural strength of silica-based ceramic cores at an ambient temperature and 1450°C improved with an increasing alumina content, whereas the opposite trend appeared at 1550°C. The creep resistances of silica-based cores were improved significantly and then slightly deteriorated with an increasing alumina content from 5% to 20%, depending on the competition effects of alumina hindering the viscous flow of liquid silica (favorable), but suppressing the devitrification rate (unfavorable). The results of this work show that silica-based cores need to follow different compositional design principles for equiaxed and columnar/single-crystal turbine blade castings.     

Mechanical and kinetic studies on the refractory fused silica of integrally cored ceramic mold fabricated by additive manufacturing

A refractory fused silica based integrally cored ceramic mold, the ceramic core with a ceramic mold shell in a single patternless construction, is fabricated by ceramic stereolithography of additive manufacturing. Refractory ceramic molds should satisfy the following restrictions such as similar strength to that of cast metal during solidification, thermal stability for dimensional accuracy, and easy removal of core after casting. Here, we report mechanical and transformation kinetic studies on the refractory fused silica of integrally cored ceramic mold. The flexural strength of sintered silica continually increases with higher density of better densification up to 11.4 MPa at 1300 °C, while it decreases from 11.3 MPa at 1350 °C to 4.6 MPa at 1500 °C. The degradation of the flexural strength is related to the larger amount of the cristobalite and microcracks generated by the abrupt contraction induced during the transformation of beta to alpha cristobalite. Given the quantitative x-ray diffraction study on transformation kinetics, an apparent activation energy Q is 674 ± 53 kJ/mol and the average time exponent 1.85, suggesting that the transformation kinetic is controlled by 1-dimensional interfacial growth.     

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.     

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.     

Reinforcement of silica-based ceramic cores based on amorphous and polycrystalline mullite fibers

In the investment casting of turbine blades, ceramic cores are key components to form complex hollow structures. Superior mechanical property and leaching rate are demanded for ceramic cores. Herein, ceramic cores were fabricated using fused silica powders as the matrix, and amorphous and polycrystalline mullite fibers as the reinforcement phases, respectively. The microstructure and property evolution of ceramic cores rely on the crystallization degree of mullite fibers are explored. Both of the mullite fibers lead to improved crystallization of cristobalite, reduced sintering shrinkage, increased apparent porosity, and benefited bending strength, creep resistance, and leaching rate of the cores. Compared to the polycrystalline mullite fibers, the amorphous fibers are metastable with large quantities of structural defects, promoting the diffusion mass transfer and forming strong interface between fibers and matrix. Therefore, the amorphous fibers have larger promotion on the bending strength and resistance to creep deformation of ceramic cores. Moreover, the structural defects of amorphous fibers ensures the high chemical activity in alkaline solutions and exhibits excellent leaching rate. The ceramic core with 4.5 wt% of amorphous mullite fibers exhibits excellent comprehensive performance with bending strengths of 28.9 MPa and 23.8 MPa at room temperature and 1550 °C, creep deformation of 0.3 mm, and leaching rate of 1.4 g/min, well meeting the casting requirements of hollow blades.     

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%.     

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.     

Investigation of microstructure and properties in short carbon fiber reinforced silica-based ceramic cores via atmosphere sintering

Short carbon fiber (C_sf) reinforced silica-based ceramic cores for investment casting were prepared by an injection molding approach and sintered in air and N₂ atmospheres, respectively. SEM and XRD results present that there are some in-situ formed silicon carbides (SiC) in sintered samples. Moreover, as for the ceramic cores sintered in N₂ atmosphere, the peaks in XRD patterns related to the cristobalite increase with an increment in C_sf content, which may be attributed to the adhesion interface provided by the C_sf and the decreased crystallization free energy. Interestingly, the sample sintered in N₂ exhibits a higher flexural strength about 16.2 MPa, which is 155 % times than that of the samples sintered in air. This is originated from an obvious composite coating consisting of fused silica, SiC and cristobalite on the C_sf. In addition, the sintering necks can further enhance the interfacial bonding strength between the fibers and ceramic cores matrix.     

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.     

Influences of mullite fibers on mechanical and thermal properties of silica-based ceramic cores

Mullite fibers composite silica-based ceramic cores were successfully prepared by injection molding. The effects of mullite fibers on the mechanical and thermal properties of ceramic cores were investigated. The results indicated that the linear shrinkage was significantly decreased and the porosity was gradually increased with the increase of mullite fibers. In addition, the flexural strength for the room temperature and the simulated casting temperature of 1500°C was increased to a maximum value when the content of mullite fibers was about 1 wt.%, and then decreased with the increase of mullite fibers. The mullite fibers of 1 wt.% presented excellent mechanical properties with a linear shrinkage of .65%, a porosity of 6.96%, and a flexural strength of 17 MPa at room temperature and 34.83 MPa at the simulated casting temperature of 1500°C. Besides, the change in microstructure and properties in various contents of mullite fibers were analyzed.     

Experimental study on high temperature performances of silica-based ceramic core for single crystal turbine blades

Silica-based ceramic cores are widely utilized for shaping the internal cooling canals of single crystal superalloy turbine blades. The thermal expansion behavior, creep resistance, and high temperature flexural strength are critical for the quality of turbine blades. In this study, the influence of zircon, particle size distribution, and sintering temperature on the high-temperature performance of silica-based ceramic cores were investigated. The results show that zircon is beneficial for narrowing the contraction temperature range and reducing the shrinkage, improving the creep resistance and high-temperature flexural strength significantly. Mixing coarse, medium and fine fused silica powders in a ratio of 5:3:2, not only reduced high temperature contraction, but effectively improved the creep resistance. Properly increasing the sintering temperature can slightly reduce the thermal deformation and improve the high-temperature flexural strength of the silica-based core, but excessively high sintering temperature negatively impacts the creep resistance and high-temperature flexural strength.     

Improved mechanical properties of SiB6 reinforced silica-based ceramic cores fabricated by 3D stereolithography printing

Silica-based ceramic core is an extremely critical component in the manufacture of hollow blades during investment casting. However, the traditional preparation methods rely more on the molds, and the manufacturing costs are relatively high. In this study, silica-based ceramics with silicon hexaboride (SiB₆) addition were prepared via 3D stereolithography printing. And the effects of the SiB₆ content on mechanical properties of the obtained ceramic samples were explored. As the SiB₆ content increased to 2.0 wt%, the linear shrinkage gradually decreased, while the room temperature and high temperature flexural strength were enhanced at the SiB₆ content from 0 to 1.0 wt% and reduced as the SiB₆ content further rose. As the SiB₆ content increased to 1.0 wt%, the linear shrinkage was reduced to 1.86% resulting from the oxidation reaction of SiB₆. Furthermore, with 1.0 wt% SiB₆ addition, the flexural strength of the samples at room temperature was enhanced from 6.75 MPa to 14.63 MPa due to the sintering promotion of oxidation product B₂O₃, and the flexural strength at 1550 °C was improved from 7.68 MPa to 13.08 MPa because of the enhanced β-cristobalite content, which is suitable for high temperature casting of ceramic cores. Therefore, it demonstrates the capability of fabricating SiB₆ reinforced silica-based ceramic cores with high performance via stereolithography.     

Microstructure and properties evolution of silicon-based ceramic cores fabricated by 3D printing with stair-stepping effect control

A ceramic core is the key component in the manufacture of the hollow turbine blades of aeroengines. Compared with the traditional injection molding method, 3D printing is more suitable for manufacturing ceramic cores with a complex geometry at high precision. However, the stair-stepping effect is inevitable in the 3D printing process and affects the surface roughness and strength of the ceramic core. In this study, to explore the influence of nano-silica content on the microstructure and properties of the ceramic core, silicon-based ceramic cores were fabricated with the addition of nano-silica powder by digital light processing and subsequent sintering at 1200 °C. The results showed that the apparent porosity and pore size of the ceramic core gradually decreased as both the nano-silica powder content and bulk density increased. Meanwhile, the printing interlayer spacing was significantly reduced, resulting in a low surface roughness, high flexural strength, and creep-resistance. To simulate the entire casting process of a superalloy blade, the thermal deformation behavior of the ceramic core was observed by heating and cooling cycles performed in a thermal dilatometer at 1540 °C. The total linear shrinkage decreased as the nano-silica powder content increased, which was mainly due to the phase transformation of cristobalite and the densification of the ceramic core sintered at 1200 °C. The low surface roughness and linear shrinkage as well as high flexural strength of the ceramic core can contribute to the excellent quality of cast superalloy blades.     

Effect of synergism of solid loading and sintering temperature on microstructural evolution and mechanical properties of 60 vol% high solid loading ceramic core obtained through stereolithography 3D printing

Solid loading has a significant effect on the curing behavior of slurry and the microstructure and properties of the ceramic core. A high-solid loading slurry can effectively improve the sintering densification of ceramic particles and improve the interlayer bonding strength and mechanical properties at both 25 °C room and higher temperatures. Herein, based on the photopolymerization theory of ceramic slurry, the solid loading was increased from 45 to 60 vol% by adjusting the composition ratio of the resin ceramic powder. Additionally, the optimal sintering temperature of the 60 vol% solid loading ceramic core was 1200 °C. The synergistic effect of the solid loading and sintering temperature controls the sintering shrinkage of the sample within 3.2%; the porosity, high temperature, and room temperature flexural strength were approximately 30%, 24 MPa, and 10 MPa, respectively. The printing preparation of high-solid loading ceramic cores can be used to guide optimizing process parameters on an industrial scale.     

Microstructure evolution and mechanical properties of ceramic shell moulds for investment casting of turbine blades by selective laser sintering

Ceramic shell moulds fabricated by traditional shell-making technology have relatively low strength, and often crack during the casting process due to the low strength. In addition, the traditional shell-making process requires long period and high cost. In this work, qualified mullite ceramic shell moulds with enhanced strength were fabricated by selective laser sintering (SLS) combined with high-temperature sintering process. The effects of SLS process parameters on dimensions were investigated, and process optimization was proposed by orthogonal experiments. The effect of sintering temperature on strength at room temperature and 900?°C were studied. X-ray diffraction analysis (XRD) and scanning electron microscopy (SEM) analysis suggested that mullitization behavior was influenced by sintering temperature. Furthermore, the content of mullite phase, mullite grain sizes, and mean length-diameter ratio of the mullite grains increased with the sintering temperature. Mechanical testing results showed that the samples sintered at 1610?°C had an excellent compressive strength of 99.01?MPa at room temperature and over 172.02?MPa at 900?°C. These values far exceed those of ceramic shell moulds fabricated by the traditional shell-making process (40.43?MPa).     

Experimental study on mechanical properties of silica-based ceramic core for directional solidification of single crystal superalloy

The effects of holding time in Bridgman furnace on mechanical properties of injection molded silica-based ceramic cores for directional solidification of SX superalloy have been investigated. The cylindrical samples (S0) were sintered at 1000 ℃ for 60 min, and some of the sintered samples (S1, S2, S3) were treated by heat treatment at 1500 ℃ to simulate the directional solidification process. Isothermal uniaxial compression tests of ceramic core samples were conducted on a Gleeble-1500D mechanical simulator. Weibull approach was used to describe the strength distribution of silica-based ceramic cores. As a result, the mean compressive strength of the sample (S0) is 40.43 MPa. The mean compressive strengths of the samples (S1, S2, S3) with heat treatment at 1500 ℃ are 54.34 MPa, 53.60 MPa and 53.81 MPa, respectively, which are significantly larger than that of S0. The mean elastic moduli of the samples (S1, S2, S3) with heat treatment at 1500 ℃ are 2726.39 MPa, 2855.91 MPa and 2797.14 MPa, respectively, which is significantly higher than that of S0. The refractory particle evolution of the ceramic core during the directional solidification process is analyzed, and the microstructural investigations show that the crack propagation of ceramic core sintered at 1000 ℃ is mainly through the sintering necks between particles. However, the crack propagation of ceramic core holding at 1500 ℃ is extended through the entire large particles. The re-sintering process of ceramic core holding at 1500 ℃ compensates the negative effect of cracks due to the volume contraction during β- to α-phase transformation and the rapid cooling process, and improves the ceramic core uniformity and mechanical properties.     

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.