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.     

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.     

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.     

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.     

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.     

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.     

Optimal Composition of Zircon–Fused Silica Ceramic Cores for Casting Superalloys

The dependence of flexural strength on crystalline phase content, residual porosity, and sintering temperature has been investigated for ceramic cores based on a mixture of fused silica and zircon. The rule of binary particle mixture, adopted for three particle sizes of fused silica, predicts a critical weight fraction of fine (zircon) particles of 46.9 wt% for the best packing. However, the optimal composition of a 37.8 wt% zircon–fused silica mixture for the flexural strength of ceramic cores found experimentally is lower in zircon content. The content of α-cristobalite +α-quartz crystallized from infilling silica sols exceeds ∼3 wt% when the strength decreases from ∼10 MPa to ∼6 MPa in samples sintered at 899–927°C. The degradation is ascribed to microcracking and the loss of coherency between the fused silica grains and the infilled silica due to β- →α-phase transformation on cooling and differential densification during sintering.     

Physical and mechanical properties of hexagonal boron nitride ceramic fabricated by pressureless sintering without additive

Hexagonal boron nitride hBN ceramic was successfully fabricated by pressureless sintering at 2100C using submicrometre hBN powders without any sintering additive. The as-prepared hBN ceramic showed a room temperature flexural strength of 30.7MPa. Its flexural strength increased with the increment of temperature in N₂ atmosphere, and it retained a strength of 57.2MPa nearly two times of the room temperature strength at 1600C due to clean grain boundaries with no glassy phase. Additionally, the as-prepared hBN ceramic showed a high thermal conductivity of 31.76Wm¹k¹ and a good thermal shock resistance, which retained a relatively high residual flexural strength of 22.6MPa 73.5 of the original flexural strength at T800C. The as-prepared hBN ceramic presents a good application prospect at high temperature.     

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.     

Additive manufacturing of Al2O3 ceramic core with applicable microstructure and mechanical properties via digital light processing of high solid loading slurry

Ceramic cores are essential intermediate mediums in casting superalloy hollow turbine blades. The developing of additive manufacturing (AM) technology provides a new approach for the preparation of ceramic cores with complex structure. In this study, alumina oxide (Al₂O₃) ceramic cores with fine complex geometric shapes were fabricated by digital light processing (DLP) in high resolution. The maximum solid content of 70 vol% of ceramic slurry was adopted in the printing process, which is important for the regulation of deformations and mechanical properties. The effects of the printing parameters, including exposure intensity, printing layer thickness and sintering temperature on the microstructures and mechanical properties of printed samples were investigated. The decrease of residual stress and similar shrinkage in X, Y, and Z directions could be obtained by adjusting the printing parameters, which are crucial to prepare complex ceramic cores with high quality. Besides, the flexure strength and open porosity of ceramic cores reached 34.84 MPa and 26.94%, respectively, which were supposed to meet the requirement of ceramic cores for the fabrication of superalloy blades.     

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.     

红柱石基刚玉-莫来石复相陶瓷的显微结构及性能

以红柱石颗粒为主要骨料,辅以莫来石颗粒和刚玉颗粒,硅微粉、铝微粉为基质料,经混合、困料及成型后,经不同温度下烧成4h,制得莫来石基刚玉-莫来石复相陶瓷,分析了烧成温度对复相陶瓷的物相组成、显微结构、烧成性能、力学性能及热学性能。结果表明:红柱石在高温下转化成针状和柱状莫来石改善复相陶瓷的烧成性能和抗热震性能;在1480℃烧成时,红柱石刚玉-莫来石复相陶瓷具有优越性能,其抗折强度为15.4MPa,耐压强度为91.6MPa,热膨胀系数为5.5×10-6/K,1100℃下水冷的抗热震次数达到99次。     

Effect of TiO2 addition on microstructure and mechanical properties of alumina-based cores prepared by sol-gel method

Alumina-based ceramic cores have widespread applications especially in the investment casting of turbine blades due to chemical inertness with most of the superalloys, capability of machining in the green state, and their mechanical stability at high temperatures. The present work studied the effects of TiO₂ addition to the alumina-based cores. These cores were prepared via the sol-gel method process by mixing alumina powders with NH₄Cl and silica sol. The effects of adding different amounts of titania from 5 to 30 wt% and different sintering procedures on mechanical, physical, thermal, chemical, and microstructural features of the bodies were investigated. According to the results of rheology measurements of the slurries and flexural strength of the green bodies, the suitable amount of solid loading was 45 vol. %. The results showed that there is an optimum content for TiO₂ addition. The specimen contained 15 wt. % titania and sintered at 1400°C for 2 hours had the thermal expansion coefficient as low as 4.8 × 10⁻⁶/°C (25-900°C), suitable mechanical properties as a result of tialite formation, and apparent porosity of 28 vol. %, respectively. The result of creep deformation test showed that this specimen had near zero deformation at 1650°C.     

Gelcasting of alumina based ceramic cores containing yttria for single crystal and directional solidification blades

Abstract

Ceramic cores play an essential role in investment casting. In this paper, gelcasting process has been successfully employed to fabricate alumina based ceramic cores containing yttria for single crystal and directional solidification blades. Based on an investigation of the formability of different ceramic slurries, material compositions of ceramic cores are determined by experiments. A proper sintering process is developed to get low sintered shrinkage, high apparent porosity and high room temperature flexural strength. The high temperature properties of ceramic cores are improved by dipping in water based yttria sol and resintering. The test results show that comprehensive properties of alumina based ceramic cores containing yttria fabricated by gelcasting are better than those of AC-1 ceramic cores made by the Beijing Institute of Aeronautical Materials, China, and that the ceramic cores can be applied to single crystal and directional solidification blade casting.     

Microstructure and mechanical properties of 3D-printed nano-silica reinforced alumina cores

Ceramic cores are an important component in the preparation of hollow turbine blades for aero-engines. Compared with traditional hot injection technology, 3D printing technology overcomes the disadvantages of a long production cycle and the difficulty in producing highly complex ceramic cores. The ceramic cores of hollow turbine blades require a high bending strength at high temperatures, and nano-mineralizers greatly improve their strength. In this study, nano-silica-reinforced alumina-based ceramic cores were prepared, and the effects of nanopowder content on the microstructure and properties of the ceramic cores were investigated. Alumina-based ceramic cores contained with nano-silica were prepared using the vat photopolymerization 3D printing technique and sintered at 1500 °C. The results showed that the linear shrinkage of ceramic cores first increased and then decreased as the nano-silica powder content increased, and the bending strength showed the same trend. The fracture mode changed from intergranular to transgranular. The open porosity and bulk density fluctuated slightly. The weight loss rate was approximately 20%. When the nano-silica content was 3%, the bending strength reached a maximum of 46.2 MPa and 26.1 MPa at 25 °C and 1500 °C, respectively. The precipitation of the glass phase, change in the fracture mode of the material, pinning crack of nanoparticles, and reduction of fracture energy due to the interlocking of cracks, were the main reasons for material strengthening. The successful preparation of 3D printed nano-silica reinforced alumina-based ceramic cores is expected to promote the preparation of high-performance ceramic cores with complex structures of hollow turbine blades.     

Effects of ZrSiO4 content on properties of SiO2-based ceramics prepared by digital light processing

SiO₂-based ceramic cores are widely used in the preparation of gas turbine engine hollow blades due to their excellent chemical stability and easy removal after casting. In this paper, ZrSiO₄ reinforced SiO₂-based ceramics were fabricated using digital light processing (DLP) technology. The results showed that the addition of ZrSiO₄ reduced the cure depth due to its high UV light absorptivity and refractive index. When the content of ZrSiO₄ increased to 15 wt%, the cristobalite content reached the maximum, and radial shrinkage reached the minimum of 1.4%. ZrSiO₄ grains could hinder the propagation of cracks, enhancing the room-temperature flexural strength. At 1550 °C, fracturing across SiO₂ grains in SiO₂-based ceramics led to the great improvement of high-temperature flexural strength. When the content of ZrSiO₄ reached 15 wt%, the flexural strength at room temperature and high temperature was 11.5 MPa and 36.7 MPa, respectively. Therefore, the SiO₂-based ceramics prepared using DLP technology have good room temperature and high temperature properties, and are expected to be used for hollow blade casting.     

The role of zircon particle size distribution, surface area and contamination on the properties of silica-zircon ceramic materials

Zircon is used as an additive to silica ceramics for use in investment casting to improve their high temperature properties. However, little is known about the mechanisms by which this occurs. To investigate the effect of zircon addition to a silica ceramic a number of silica-zircon formulations were created utilising three different batches of zircon with different particle size distributions (PSDs), surface areas and contaminant inclusions. The contaminant inclusion of the zircon, present in the zircon from the ball-milling stage of manufacture, appeared to have a large effect on the room temperature flexural strength, high temperature flexural strength and high temperature creep properties. It is also suggested that any increase in post-fired cristobalite content and any change to crystal growth morphology was due to the inherent contaminant inclusions and not because of the zircon itself. Hence, use of silica-zircon materials in ceramics for investment casting should account for variation in the contaminant inclusion of the zircon in order to maintain the specific material properties required.     

Effects of different types of sintering additives and post-heat treatment (PHT) on the mechanical properties of SHS-fabricated Si3N4 ceramics

Porous silicon nitride (Si₃N₄) ceramics were fabricated by self-propagating high temperature synthesis (SHS) using Si, Si₃N₄ and sintering additive as raw materials. Effects of different types of sintering additives with varied ionic radius (La₂O₃, Sm₂O₃, Y₂O₃, and Lu₂O₃) on the phase compositions, development of Si₃N₄ grains and flexural strength (especially high-temperature flexural strength) were researched. Si₃N₄ ceramics doped with sintering additive of higher ionic radius had higher average aspect ratio, improved room-temperature flexural strength but degraded high-temperature flexural strength. Besides, post-heat treatment (PHT) was conducted to crystallize amorphous grain boundary phase thus improving the creep resistance and high-temperature flexural strength of SHS-fabricated Si₃N₄ ceramics. Excellent high-temperature flexural strength of 140 MPa~159 MPa and improved strength retention were achieved after PHT at 1400 °C.