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.     

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.     

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.     

Silica strengthened alumina ceramic cores prepared by 3D printing

Ceramic cores based on alumina and silica are important in the manufacturing of hollow blades. However, obtaining good properties and precision is still challenging. In this research, alumina-based ceramics cores were obtained by 3D printing technology, and the effects of silica contents on the mechanical properties of the as-obtained alumina ceramic cores were evaluated. The results showed significant improvements in flexural strengths of the ceramics from 13.3 MPa to 46.3 MPa at silica contents from 0 wt% to 30 wt% due to formation of mullite phase (Al₆Si₂O₁₃). By contrast, the flexural strengths declined as silica content further increased due to the generation of massive liquid phase. Also, porous structures and cracks were observed by scanning electron microscopy due to the removal of cured photosensitive resin and the mullitization reaction between alumina and silica, respectively. The manufacturing process of hollow blades required ceramic cores with flexural strengths greater than 20 MPa to resist the strike of metal liquid, as well as open porosity above 20 % to provide space for alkali liquor to dissolve the ceramic cores. As a result, 10 wt% silica was determined as the optimal value to yield ceramics with improved properties in terms of flexural strength (35.6 MPa) and open porosity (47.5 %), thereby satisfy the application requirement for the fabrication 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%.     

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.     

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.     

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.     

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.     

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.     

Effect of zirconia content and particle size on the properties of 3D-printed alumina-based ceramic cores

Alumina-based ceramic cores are used to manufacture the internal structures of hollow alloy blades, requiring both high precision and moderate properties. In this work, zirconia is regarded as a promoter to improve the mechanical properties of sintered ceramic. The effect of zirconia content and particle size on the microstructure and mechanical properties of ceramics was evaluated. The results indicate that the flexural strength of sintered ceramics reached the maximum of 14.5 ± 0.5 MPa when 20 wt% micron-sized (10 μm) zirconia (agglomerate size, consistent with the alumina particle size) was added, and 26.5±2.5 MPa when 15 wt% 0.3 μm zirconia was added. Zirconia with submicron-sized (0.3 μm) particles effectively filled the pores between alumina particles, thus leading to the maximum flexural strength with a relatively low content. The corresponding sintered ceramics had a bulk density of 2.0 g/cm³ and open porosity of 59.6%.     

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.     

MgO-TiO_2-La_2O_3系氧化铝陶瓷的力学性能及物相分析

采用MgO-TiO2-La2O3为烧结助剂,利用低温烧结技术制备95氧化铝瓷。研究了烧成温度和助剂含量对氧化铝陶瓷力学性能及物相组成的影响。结果表明:在MgO含量为1.5wt%,TiO2为1.0wt%,La2O3为2.5wt%,1500℃保温2h可得到抗弯强度和硬度分别为348.94MPa和79.6HRA的氧化铝陶瓷。     

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.     

Study on Gelcasting of Fused Silica Glass Using Glutinous Rice Flour as Binder

Gelcasting is a colloidal processing method for fabricating high-strength and complex shape ceramic green bodies. However, industry has been reluctant to use the gelcasting technique because the most commonly used gel, acrylamide (AM), is a neurotoxin. Here, we report an attempt at the gelcasting of fused silica glass using a natural and nontoxic gel, glutinous rice flour (GRF) as binder. The GRF-based aqueous system was found to behave excellently in the gelcasting process. Flexural strength of fused silica green bodies solidified with only 3 wt% GRF is up to 11.87 MPa. Bulk density and flexural strength of fused silica glass sintered at 1275 °C are 1.75 g/cm³ and 47.02 MPa, respectively.     

Effect of magnesia-alumina spinel precursor sol on the sintering property of fused magnesia refractory

The sintering property of fused magnesia refractory was investigated by the fused magnesia powder as matrix and the synthetic magnesia-alumina spinel precursor sol as binder. The spinel precursor sol was prepared by co-precipitation method and was characterized by its particle size, thermal analysis, microstructure, phase development with temperatures, and so on. The effect of spinel precursor sol on the sintering property of fused magnesia refractory were studied after heat treatment at 1450?°C and 1550?°C. The results showed that the bulk density, flexural strength and linear shrinkage of the sintered samples firstly increase and then decrease with increasing spinel precursor sol. The bulk density and flexural strength (cold modulus of rupture) of the sample sintered at 1550?°C, introduced with 1?wt% spinel precursor sol, reached 3.10?g/cm³ and 47.25?MPa, respectively. From the experimental results, magnesia-alumina spinel precursor sol can replace the traditional binders and improve the sintering property of fused magnesia products.     

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.     

Fabrication and characterization of silica ceramic compact prepared using Aloe-Vera mucilage as a binder

In this study, silica compacts were fabricated through a powder processing route at different compaction pressure, using Aloe-Vera (AV) mucilage as a binder. The silica compacts were prepared at 90, 100, and 110 MPa compaction pressure using 0%–16 wt% of AV binder. The optimum amount of AV binder was 14 wt% for both 90 and 100 MPa and 12 wt% for 110 MPa. The maximum achieved green density and green strength of silica compacts at the optimum binder amount were 62.3% and 4 MPa, respectively at 110 MPa compaction pressure. The green silica compacts prepared at 110 MPa compaction pressure exhibited a minimum porosity of 21% and maximum flexural strength of 15 MPa after sintering at 1400°C. The green silica compacts with the optimum amount of binder were strong enough for machining. The Fourier transform infrared spectroscopy analysis revealed the functional groups present in AV mucilage. The binder burnout characteristic of AV mucilage in the silica compact was determined by thermogravimetric analysis and differential thermal analysis. Additionally, AV gel acted as a binder and solvent simultaneously for ceramic compaction.     

Evolution of the microstructure and mechanical properties of stereolithography formed alumina cores sintered in vacuum

Stereolithography (SL) was used to form alumina ceramic cores. The effect of sintering temperature on the microstructure and mechanical properties of the alumina ceramics are investigated, which were sintered in vacuum. The results indicate that, as the sintering temperature increased the particle size of alumina slightly increased, and the interlayer spacing first decreased and then increased. The open porosity of alumina ceramics significantly decreased as the sintering temperature in vacuum increased. The flexural strength and hardness increased as the sintering temperature increased. When sintered at 1150 °C, the flexural strength was found to be 33.7 MPa, the shrinkage was 2.3 %, 2.4 %, and 5.3 % in the X, Y, and Z directions, respectively, and the open porosity was 37.9 %. These results are similar to those found from sintering at 1280 °C in air.     

Preparation,mechanical, and leaching properties of CaZrO3 ceramic cores

The CaZrO₃ ceramic core materials with excellent mechanical and chemical properties were successfully prepared using single-phase CaZrO₃ powders. Effects of particle size ratio and sintering temperature on the mechanical and chemical properties of CaZrO₃ ceramic core materials were researched. The chemical property was analyzed by leaching research of core materials in 10 wt% and 20 wt% HNO₃ solution at the boiling point. Results showed that the suitable particle size ratio was important for the preparation of CaZrO₃ ceramic core materials with excellent comprehensive properties. The addition of fine particles in ceramic core materials promoted the densification process owing to the framework formed by coarser particles and sintering neck formed by fine particles between coarse particles, which was beneficial for further improving their bending strength. When the content of particles with 200 mesh size was 80wt%, the highest bending strength was obtained, 54.38 ± 5.28 MPa. The porosity was 17.45% and the volume density was 3.86 g/cm³. The increasing sintering temperature increased the densification of CaZrO₃ ceramic core materials by offering the sintering driving force, further leading to the improvement of bending strength. When the temperature was 1650℃, at the 20% content of particles with 200 mesh size, the highest bending strength of CaZrO₃ cores reached 51.01 ± 5.18 MPa. Meanwhile, the porosity was 18.65% and the volume density was 3.83 g/cm³. Additionally, the CaZrO₃ samples could be effectively leached in 10 wt% HNO₃ solution. Therefore, CaZrO₃ materials with good mechanical and leaching properties were believed to be a suitable candidate for ceramic core materials in the investment casting of alloys with high melting point.