Enhanced mechanical properties of 3D printed alumina ceramics by using sintering aids

Stereolithography based 3D printing provides an efficient pathway to fabricate alumina ceramics, and the exploration on the mechanical properties of 3D printed alumina ceramics is crucial to the development of 3D printing ceramic technology. However, alumina ceramics are difficult to sinter due to their high melting point. In this work, alumina ceramics were prepared via stereolithography based 3D printing technology, and the improvement in the mechanical properties was investigated based on the content, the type and the particle size of sintering aids (TiO₂, CaCO₃, and MgO). The flexural strength of the sintered ceramics increased greatly (from 139.2 MPa to 216.7 MPa) with the increase in TiO₂ content (from 0.5 wt% to 1.5 wt%), while significant anisotropy in mechanical properties (216.7 MPa in X-Z plane and 121.0 MPa in X–Y plane) was observed for the ceramics with the addition of 1.5 wt TiO₂. The shrinkage and flexural strength of the ceramics decreased with the increase in CaCO₃ content due to the formation of elongated grains, which led to the formation of large-sized residual pores in the ceramics. The addition of MgO help decrease the anisotropic differences in shrinkage and flexural strength of the sintered ceramics due to the formation of regularly shaped grains. This work provides guidance on the adjustment in flexural strength, shrinkage, and anisotropic behavior of 3D printed alumina ceramics, and provides new methods for the fabrication of 3D printed alumina ceramics with superior mechanical properties.     

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.     

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%.     

Microstructures and mechanical properties of functionally graded TiCN–TaC ceramics prepared by a novel layer processing strategy

Functionally graded TiCN–TaC ceramics (FGTTCs) were fabricated using a novel layer processing method based on a vacuum hot-press sintering technology. Microstructural investigations revealed a visibly layered structure for the FGTTCs with relatively flat boundaries between the neighboring layers; additionally, the layer thickness was facilely controlled. With an increase in the sintering temperature, the hardness and flexural strength of the surface and middle layers of the FGTTCs initially increased, and then decreased. The fracture toughness of the surface layer did not undergo significant changes after sintering at various temperatures, except at 1500 °C. The FGTTC sintered at 1350 °C contained uniform fine grains and simultaneously exhibited transgranular and intergranular fracture modes. Further, it presented excellent comprehensive mechanical properties, i.e., surface layer hardness = 20.28 ± 0.18 GPa, flexural strength = 1553.76 ± 22 MPa, surface layer fracture toughness = 7.29 ± 0.24 MPa m^1/2. Under the same sintering conditions, our FGTTCs presented superior mechanical properties against homogeneous TiCN–TaC ceramics (HTTCs), achieving a considerably higher flexural strength (1553.76 ± 22 vs 953.35 ± 24 MPa).     

Effect of printing parameters on mechanical properties of extrusion-based additively manufactured ceramic parts

The purpose of this study is to investigate the effect of printing parameters on the physical and mechanical properties of additively manufactured ceramics (alumina and zirconia). Sample parts were obtained by extrusion-based additive manufacturing of a ceramic-binder mixture and subsequent post-processing (debinding and sintering). Their mechanical properties (microhardness, flexural strength, toughness) were measured and correlated with the printing parameters. Part orientation is the most significant factor for microhardness and flexural strength in both ceramic materials. Parts with vertical orientation show higher hardness while horizontal samples show higher flexural strength compared to their respective counterparts. Extrusion velocity was found to be insignificant for hardness and flexural strength. However, a marginal increase in fracture toughness with the increase in the extrusion velocity was observed. The fracture toughness of additively manufactured ceramics shows an increasing trend with elastic modulus and flexural strength and a decreasing trend with hardness and sintered density.     

Properties of multiple oxide-bonded porous SiC ceramics prepared by an infiltration technique

Multiple oxide-bonded porous SiC ceramics were fabricated by infiltrating a porous powder compact of SiC and alumina with cordierite sol followed by sintering at 1300-1400°C in air for 3 hours. The microstructures, phase components, mechanical properties, and air permeation behavior of the developed porous ceramics were examined and compared with materials obtained by the traditional powder processing route. The porosity, average pore diameter, and flexural strength of the ceramics varied from 33 to 37 vol%, ~12-14 μm and ~23-39.6 MPa, respectively, with variation in sintering temperature. The X-ray diffraction results reveal that both the amount of cordierite and mullite as the binder increased with increase in sintering temperature. In addition, it was found that the addition of alumina in powder form effectively enhanced the strength due to formation of mullite in the bond phase in contrast to the samples prepared without alumina additive. To determine the suitability of the material in particulate filtration application, particle collection efficiency of the filter material was evaluated theoretically using single collector efficiency model.     

3D printing of porous scaffolds BaTiO3 piezoelectric ceramics and regulation of their mechanical and electrical properties

A series of porous scaffolds of piezoelectric ceramic barium titanate (BaTiO₃) were successfully fabricated by Digital Light Processing (DLP) 3D printing technology in this work. To obtain a high-precision and high-purity sample, the debinding sintering profile was explored and the optimal parameters were determined as 1425 °C for 2h. With the increase of scaffolds porosity from 10% to 90%, the compressive strength and piezoelectric coefficient (d₃₃) decreased gradually. The empirical formulas about the mechanical and piezoelectric properties were obtained by adjusting BaTiO₃ ceramics with different porosity. In addition, the distribution of potential and stress under 100 MPa pressure were studied by the finite element method (FEM).     

Fabrication and characterization of anorthite–mullite–corundum porous ceramics from construction waste

In this work, anorthite–mullite–corundum porous ceramics were prepared from construction waste and Al₂O₃ powders by adding AlF₃ and MoO₃ as mineralizer and crystallization catalyst, respectively. The effects of the sintering temperature and time on open porosity, mechanical properties, pore size distribution, microstructure, and phase composition were characterized in detail. The results showed that the formation of the mullite whiskers and the properties of the anorthite–mullite–corundum porous ceramics depended more on the sintering temperature than the holding time. By co-adding 12 wt% AlF₃ and 4 wt% MoO₃, mullite whiskers were successfully obtained at sintering temperatures upon 1350 °C for 1 h. Furthermore, the resultant specimens exhibited excellent properties, including open porosity of 66.1±0.7%, biaxial flexural strength of 23.8±0.9 MPa, and average pore size of 1.32 µm (the corresponding cumulative volume percent was 37.29%).     

Influence of resin composition on rheology and polymerization kinetics of alumina ceramic suspensions for digital light processing (DLP) additive manufacturing

Alumina ceramics with optimized microstructures and mechanical properties were obtained by the attractive digital lighting processing (DLP) additive manufacturing methodology in the present study. A acrylate-based resin system was designed for the alumina powders with a mean particle size of 0.5 μm. The influence of oligomer on the viscosity and polymerization kinetics of the ceramic suspensions has been elaborately discussed by rheology, curing depth and photo-DSC characterizations. The results indicated that the introduction of oligomer has improved the cross-linking density of resins and decreased the critical dose of energy for resin polymerization, which contributed to a tougher ceramic-resin slice with higher dimensional accuracy. Densifying processes including debinding and high temperature sintering of the ceramic parts were conducted according to the TG-DTA characterizations, alumina ceramics with uniform microstructures and eliminated delamination or intralaminar cracks were finally obtained. The flexural strength was 471 MPa for the ceramics obtained from the resin composition containing 20 wt% oligomer, Weibull modulus for the ceramics were determined to be 17.31 by evaluating thirty all sides polished ceramics, indicating the highly uniform property of the ceramics fabricated by DLP additive manufacturing.     

High-Strength Porous Alumina Ceramics by the Pulse Electric Current Sintering Technique

High-strength porous alumina has been fabricated with a microstructure control using the pulse electric current sintering (PECS) technique. During sintering the discharge, which is assumed to take place in the voids between the particles, is thought to promote the bridging of particles by neck growth in the initial stages of sintering, leaving high porosity. The effect of dopants (MgO, 200 ppm; TiO₂, 1000 ppm) and of secondary inclusions (3 vol% 3Y-TZP) on the constrained densification and the improvement in the mechanical behavior of porous alumina ceramics has been reported. The porosity of the fabricated porous alumina was controllable between 30% and 50% depending on the sintering temperature. The flexural strength of alumina having 30% and 42% porosity showed impressive values of 250 and 177 MPa, respectively. The dominance of the preferential neck growth of grains over densification significantly improved the mechanical properties of porous alumina, besides leaving high porosity.     

In situ synthesis,mechanical properties,and microstructure of reactively hot pressed WB4 ceramic with Ni as a sintering additive

In this study, tungsten tetraboride (WB₄) ceramics were synthesized in situ from powder mixtures of W and amorphous B with Ni as a sintering aid by reactive hot pressing method. The as-synthesized ceramics exhibited porosity as low as 0.375% and ultra-high Vickers hardness (H_v), as much as 49.808?±?1.683?GPa (for the low load of 0.49?N). It was seen that the addition of Ni greatly improved the sinterability of WB₄ ceramic. Besides, the flexural strength and fracture toughness of WB₄ ceramic were measured for the first time to be 332.857?±?36.763?MPa and 4.136?±?0.259?MPa?m^1/2, respectively, suggesting that the ceramic has good mechanical properties. The effects of sintering temperature and holding time on the densification, Vickers hardness, and mechanical properties of WB₄ ceramics were also investigated systematically as part of our study. The results indicated that increasing the sintering temperature can obviously improve the densification and mechanical properties of the ceramics. The bulk density and Vickers hardness of WB₄ ceramic sintered at 1650?°C for 60?min under 30?MPa revealed the highest values of 6.366?g?cm^?3 and 27.948?±?0.686?GPa (for the high load of 9.8?N), respectively. The flexural strength increased to the highest value of 332.857?±?36.763?MPa for sintering temperature up to 1550?°C, but decreased slightly as the sintering temperature further increased to 1650?°C. On the other hand, the fracture toughness increased gradually with increasing temperature. It was also found that Vickers hardness showed a similar trend as the densification of the samples with increasing temperature and holding time. Besides, no obvious improvements in the densification, mechanical properties, and Vickers hardness of the samples with sintering time were observed in this study. The microstructure and fracture behaviours of the as-synthesized WB₄ ceramic were also revealed, and the toughening mechanism has been discussed.     

Mechanical and dielectric properties of Si3N4-SiO2 ceramics prepared by digital light processing based 3D printing and oxidation sintering

Si₃N₄-SiO₂ ceramics are considered as the preferred high-performance wave-transmitting material in the aerospace field. However, traditional fabrication methods for Si₃N₄-SiO₂ ceramics have the disadvantages of high cost and complicated fabrication process. In this paper, Si₃N₄-SiO₂ ceramics with excellent mechanical and dielectric properties were fabricated by digital light processing-based 3D printing combined with oxidation sintering. Firstly, the curing thickness and viscosity of slurries with different solid loadings for vat photopolymerization-based 3D printing were studied. Then, the effects of the sintering temperature on the linear shrinkage, phase composition, microstructure, flexural strength, and dielectric properties of Si₃N₄-SiO₂ ceramics, and the influences of solid loading on them were explored. The curing thickness and viscosity of the slurry with a solid loading of 55 vol% were 30 μm and ∼1.5 Pa‧s, respectively. The open porosity and the flexural strength of Si₃N₄-SiO₂ ceramic with a solid loading of 55 vol% were 4.3 ± 0.61% and 76 ± 5.6 MPa, respectively. In the electromagnetic wave band of 8–18 GHz, the dielectric constant of Si₃N₄-SiO₂ ceramics was within the range of less than 4, and the dielectric loss remained below 0.09. The method of digital light processing-based 3D printing combined with oxidation sintering can be further extended in the preparation of Si₃N₄-based structure-function integrated ceramics.     

Influence of injection temperature and pressure on the properties of alumina parts fabricated by low pressure injection molding (LPIM)

The quality of ceramics parts made by powder injection molding (PIM) method is influenced by a range of factors such as powder and binder characteristics, rheological behavior of feedstock, molding parameters and debinding and sintering conditions. In this study, to optimize the molding parameters, the effect of injection temperature and pressure on the properties of alumina ceramics in the LPIM process were thoroughly studied. Experimental tests were conducted on alumina feedstock with 60 vol% powder. Injection molding was carried out at temperatures and pressures of 70–100 °C and 0.1–0.6 MPa respectively. Results showed that increase in injection temperature and pressure and the resulting increase in flow rate leads to the formation of void which impairs the properties of molded parts. The SEM studies showed that injection at temperature of 100 °C results in evaporation of binder components. From the processing point of view, the temperature of 80 °C and pressure of 0.6 MPa seems to be the most suitable condition for injection molding. In addition, the effects of sintering conditions (temperature and time) on the microstructure and mechanical properties are discussed. The best final properties were found using injection molding under the above stated conditions, thermal debinding and sintering at 1700 °C during 3 h.     

Effects of particle size distribution and sintering temperature on properties of alumina mold material prepared by stereolithography

Alumina mold materials prepared by stereolithography usually have considerable sintering shrinkage, and their properties related to casting have been rarely studied. In this study, alumina molds materials were prepared by stereolithography, and the effects of particle size distribution and sintering temperature on the properties of the materials were investigated. Results show that the viscosity of the slurries decreases as the fraction of fine powder increases, and the particle size distribution affects the curing behaviors slightly. Sintering shrinkage increases as the fraction of fine powder or the sintering temperature increases. Although lower sintering shrinkage can be achieved by sintering at 1350 °C or 1450 °C, the mold materials sintered at lower temperatures would continue to shrink under the service temperature of 1550 °C, and thus 1550 °C is determined as the optimal sintering temperature. As the fraction of fine powder increases, the creep resistance first increases and then decreases, and specimens prepared with 0.1 fraction of fine powder exhibit the best creep resistance with the droop distance of 4.44 ± 0.45 mm. Specimens prepared with 0.1 fraction of fine powder and sintered at 1550 °C exhibit linear shrinkage of 6.36% along the X/Y direction and 11.39% along the Z direction, and have a flexural strength of 78.15 ± 3.50 MPa and porosity of 30.12 ± 0.08%. The resulting material possesses relatively low sintering shrinkage, proper mechanical strength, porosity and high-temperature properties that meet the requirements for casting purposes.     

Effect of carbon content on electrical,thermal, and mechanical properties of porous SiC ceramics with B4C and C additives

The electrical, thermal, and mechanical properties of porous SiC ceramics with B₄C-C additives were investigated as functions of C content and sintering temperature. The electrical resistivity of porous SiC ceramics decreased with increases in C content and sintering temperature. A minimal electrical resistivity of 4.6 × 10^?2 Ω·cm was obtained in porous SiC ceramics with 1 wt% B₄C and 10 wt% C. The thermal conductivity and flexural strength increased with increasing sintering temperature and showed maxima at 4 wt% C addition when sintered at 2000 °C and 2100 °C. The thermal conductivity and flexural strength of porous SiC ceramics can be tuned independently from the porosity by controlling C content and sintering temperature. Typical electrical resistivity, thermal conductivity, and flexural strength of porous SiC ceramics with 1 wt% B₄C-4 wt% C sintered at 2100 °C were 1.3 × 10^?1 Ω·cm, 76.0 W/(m·K), and 110.3 MPa, respectively.     

Near-net-size preparation of porous mullite matrix ceramics with in situ formed 3D mullite whisker network

Porous mullite matrix ceramics have excellent thermal and mechanical properties suitable for applications such as in thermal insulation. However, their applications are limited by processing defects from nonuniform sintering shrinkage and the trade-off between high porosity (preferred for low thermal conductivity) and high mechanical strength. Herein, we seek to minimize the sintering shrinkage by near-net-size preparation and improve the strength by in situ formed whisker network structure. Gelcasting forming technology and pressureless sintering were used to prepare porous mullite matrix ceramics using kyanite and α-Al₂O₃ powders as the starting materials and using MoO₃ to promote the growth of mullite whiskers. The results showed that the sintering shrinkage could be compensated by the volume expansion from solid-state reaction during reaction sintering. The in situ formed three-dimensional (3D) whisker network further reduced sintering shrinkage and effectively improved the strength of the ceramics. An ultralow sintering shrinkage of .78% was achieved. The near-net-shape porous mullite matrix ceramics strengthened by 3D whisker network had a high porosity of 63.9%, a high compressive strength of 83.8 MPa and a high flexural strength of 53.5 MPa.     

Porous SiC ceramics prepared via freeze-casting and solid state sintering

Porous SiC ceramics were prepared by freeze-casting process. In order to enhance the mechanical properties of the porous SiC, poly(vinyl alcohol) (PVA) was added as binder and pore morphology controller in this work. The results indicated that high porosity (>60%) SiC ceramics was obtained although the sintering temperature was over 2000 °C. The pore structure could be divided into two kinds: macropores generated by sublimation of large ice crystals, and micropores in the ceramic matrix caused by sublimating of small ice crystals, stacking of SiC particles, and burning out of PVA. With the increase of the sintering temperature, the specimens exhibited higher density, thus resulted in higher strength. Porous SiC ceramics sintered at 2100 °C showed a good flexural strength of 11.25 MPa with an open porosity as high as 66.46%.     

Rapid and uniform in-situ solidification of alumina suspension via a non-contamination DCC-HVCI method using MgO sintering additive as coagulating agent

A novel rapid, uniform and non-contamination in-situ solidification method for alumina suspension by DCC-HVCI method using MgO sintering additive as coagulating agent was reported. MgO was used to release Mg²⁺ in suspensions via reaction with acetic acid generated from glycerol diacetate (GDA) at elevated temperature as well as to improve density and suppress grain growth of alumina ceramics during sintering. Influence of adding 0.7 wt% MgO with 2.0 vol% GDA in alumina suspension on coagulation process and properties of green bodies and sintered samples were investigated. It was indicated that the controlled coagulation of the suspension could be achieved after treating at 70 °C for 10 min. Homogeneous composition distribution of Mg element in EDS result indicated the uniform solidification of suspensions. Compressive strength of wet-coagulated bodies is 2.09±0.25 MPa. Dense alumina ceramics with relative density of 99.2% and flexural strength of 354±16 MPa sintered at 1650 °C for 4 h present homogeneous microstructure. The result indicated that the novel DCC-HVCI method via a sintering additive reaction with no contamination, short coagulation time and uniform in-situ solidification is a promising colloidal forming method for preparing high-performance ceramic components with complex shape.     

High-strength TiB2-B4C composite ceramics sintered by spark plasma sintering

Spark plasma sintering (SPS) is an advanced sintering technique because of its fast sintering speed and short dwelling time. In this study, TiB₂, Y₂O₃, Al₂O₃, and different contents of B₄C were used as the raw materials to synthesize TiB₂-B₄C composites ceramics at 1850°C under a uniaxial loading of 48 MPa for 10 min via SPS in vacuum. The influence of different B₄C content on the microstructure and mechanical properties of TiB₂-B₄C composites ceramics are explored. The experimental results show that TiB₂-B₄C composite ceramic achieves relatively good comprehensive properties and exceptionally excellent flexural strength when the addition amount of B₄C reaches 10 wt.%. Its relative density, Vickers hardness, fracture toughness, and flexural strength reach to 99.20%, 24.65 ± .66 GPa, 3.16 MPa·m^1/2, 730.65 ± 74.11 MPa, respectively.     

Increasing the tensile strength of oxide ceramic matrix mini-composites by two-step sintering

Adapting conventional sintering (CS) techniques of monolithic ceramics for the production of oxide ceramic matrix composites (Ox-CMCs) comes along with a few drawbacks, such as fiber degradation. Thus, the applicability of two-step sintering (TSS) for the production of Ox-CMCs based on Nextel™ 610 fibers and porous alumina matrix is investigated in this study for the first time. Uniaxial tensile tests were performed to evaluate the performance of mini-composites produced by TSS and compared with those produced by CS. Parameters known for influencing the mechanical behavior of the mini-composites, such as grain size, porosity, shrinkage, as well as matrix properties, were analyzed. Both sintering techniques resulted in similar grain size distributions, whereas TSS showed higher total porosity and lower amount of sintering-induced cracks. As a result, TSS samples showed a higher tensile strength of 230±27 MPa when compared to 133±8 MPa for CS. In general, it was observed that most of the densification happens during the first phase of TSS, while the matrix is slowly strengthened during the second step. Therefore, the reported TSS process is a very promising and easy-to-apply heat treatment for producing Ox-CMCs with controlled microstructure.