Mechanical properties of sintered ZrB2-SiC ceramics

ZrB₂ ceramics containing 10-30 vol% SiC were pressurelessly sintered to near full density (relative density >97%). The effects of carbon content, SiC volume fraction and SiC starting particle size on the mechanical properties were evaluated. Microstructure analysis indicated that higher levels of carbon additions (10 wt% based on SiC content) resulted in excess carbon at the grain boundaries, which decreased flexure strength. Elastic modulus, hardness, flexure strength and fracture toughness values all increased with increasing SiC content for compositions with 5 wt% carbon. Reducing the size of the starting SiC particles decreased the ZrB₂ grain size and changed the morphology of the final SiC grains from equiaxed to whisker-like, also affecting the flexure strength. The ceramics prepared from middle starting powder with an equiaxed SiC grain morphology had the highest flexure strength (600 MPa) compared with ceramics prepared from finer or coarser SiC powders.     

Pressureless sintering of silicon carbide ceramics containing zirconium diboride

SiC-5 wt.% ZrB₂ composite ceramics with 10 wt.% Al₂O₃ and Y₂O₃ as sintering aids were prepared by presureless liquid-phase sintering at temperature ranging from 1850 to 1950 °C. The effect of sintering temperature on phase composition, sintering behavior, microstructure and mechanical properties of SiC/ZrB₂ ceramic was investigated. Main phases of SiC/ZrB₂ composite ceramics are all 6H-SiC, 4H-SiC, ZrB₂ and YAG. The grain size, densification and mechanical properties of the composite ceramic all increase with the increase of sintering temperatures. The values of flexural strength, hardness and fracture toughness were 565.70 MPa, 19.94 GPa and 6.68 MPa m^1/2 at 1950 °C, respectively. The addition of ZrB₂ proves to enhance the properties of SiC ceramic by crack deflection and bridging.     

Preparation,microstructure and ion-irradiation damage behavior of Al4SiC4-added SiC ceramics

Single-phase Al₄SiC₄ powder with a low neutron absorption cross section was synthesized and mixed with SiC powder to fabricate highly densified SiC ceramics by hot pressing. The densification of SiC ceramics was greatly improved by the decomposition of Al₄SiC₄ and the formation of aluminosilicate liquid phase during the sintering process. The resulting SiC ceramics were composed of fine equiaxed grains with an average grain size of 2.0 μm and exhibited excellent mechanical properties in terms of a high flexure strength of 593 ± 55 MPa and a fracture toughness of 6.9 ± 0.2 MPa m^1/2. Furthermore, the ion-irradiation damage in SiC ceramics was investigated by irradiating with 1.2 MeV Si⁵⁺ ions at 650 °C using a fluence of 1.1 × 10¹⁶ ions/cm², which corresponds to 6.3 displacements per atom (dpa). The evolution of the microstructure was investigated by X-ray photoelectron spectroscopy (XPS) and Raman spectroscopy. The breaking of Si–C bonds and the segregation of C elements on the irradiated surface was revealed by XPS, whereas the formation of Si–Si and C–C homonuclear bonds within the Si–C network of SiC grains was detected by Raman spectroscopy.     

Effects of the initial α-SiC content on the microstructure, mechanical properties, and permeability of macroporous silicon carbide ceramics

By using α- and/or β-SiC staring powders, the effects of the initial α-phase content on the microstructure, mechanical properties, and permeability of macroporous SiC ceramics were investigated. When β-SiC powder or a mixture of α/β powders containing a small amount (≤10%) of α-SiC powder was used, the microstructure consisted of large platelet grains. In contrast, when using α-SiC powder or α/β powders containing a large amount (>10%) of α powders, the microstructure consisted of small equiaxed grains. The development of large α-SiC platelet grains in the microstructure did not result in any improvement of the flexural strength of the macroporous SiC ceramics because of the accompanying pore growth and grain growth. The growth of the platelet-SiC grains was beneficial in increasing the gas permeability of the macroporous SiC ceramics from 4.12 × 10⁻¹³ m² for macroporous SiC with an equiaxed microstructure to 1.89 × 10⁻¹² m² for macroporous SiC ceramics with large platelet grains.     

Preparation of Porous Si3N4 Ceramics with Controlled Porosity and Microstructure by Fibrous α‐Si3N4 Addition

Porous silicon nitride ceramics with various porosities were fabricated by liquid phase sintering of mixtures containing fibrous and equiaxed α‐Si₃N₄ powder with a various content ratios. The effects of the contents of the fibrous α‐Si₃N₄ powder (0%–100%) on the microstructure and mechanical properties of porous Si₃N₄ ceramics were studied. As the increase of the fibrous α‐Si₃N₄ powder content, both the density of green bodies and the linear shrinkage decreased, resulting in increased porosity due to the inhibited densification by the fibrous Si₃N₄ particle. XRD analysis proved the complete formation of single β‐Si₃N₄ phase. SEM analysis revealed that the microstructure of the low content of fibrous α‐Si₃N₄ porous ceramics was almost composed of fine elongated β‐Si₃N₄ grains with high aspect ratio while numerous coarse elongated β‐Si₃N₄ grains with low aspect ratio surrounding fine grains were formed as the content of the fibrous α‐Si₃N₄ powder increased. With the increase in content of the fibrous α‐Si₃N₄ powder from 0% to 100%, the porosity changed from 47.8% to 56.6%, and the flexural strength decreased from 146 to 62 MPa correspondingly, indicating a flexural adjustment of the porosity and mechanical properties.     

Electrical,thermal, and mechanical properties of porous silicon carbide ceramics with a boron carbide additive

The effects of the boron carbide (B₄C) content and sintering atmosphere on the electrical, thermal, and mechanical properties of porous silicon carbide (SiC) ceramics were investigated in the porosity range of 58.3%–70.3%. The electrical resistivities of the nitrogen-sintered porous SiC ceramics (∼10^–1 Ω·cm) were two orders of magnitude lower than those of argon-sintered porous SiC ceramics (∼10¹ Ω·cm). Both the thermal conductivities (3.3–19.8 W·m^–1·K^–1) and flexural strengths (8.1–32.9 MPa) of the argon- and nitrogen-sintered porous SiC ceramics increased as the B₄C content increased, owing to the decreased porosity and increased necking area between SiC grains. The electrical resistivity of the porous SiC ceramics was primarily controlled by the sintering atmosphere owing to the N-doping from the nitrogen atmosphere, and secondarily by the B₄C content, owing to the B-doping from the B₄C. In contrast, the thermal conductivity and flexural strength were dependent on both the porosity and necking area, as influenced by both the sintering atmosphere and B₄C content. These results suggest that it is possible to decouple the electrical resistivity from the thermal conductivity by judicious selection of the B₄C content and sintering atmosphere.     

Microstructure and mechanical properties of carbon-precursor-added B4C and B4C−SiC ceramics subjected to pressureless sintering

Organic-carbon-precursor-added B₄C and B₄C–SiC ceramics were subjected to pressureless sintering at various temperatures. The carbon precursor increased the densification of the B₄C and B₄C–SiC ceramics sintered at 2200 °C to 95.6 % and 99.1 % theoretical density (T.D.), respectively. The pyrolytic carbon content of the B₄C–SiC composite decreased with increasing SiC content. The graphitization degree of pyrolytic carbon decreased slightly with the amount of carbon precursor and content of SiC. The 95 wt. % B₄C–5 wt. % SiC composite added with 7.5 wt. % carbon precursor and sintered at 2200 °C outperformed the other B₄C–SiC composites, and its sintered density, flexural strength, Young’s modulus, and microhardness were 98.6 % T.D., 879 MPa, 415 GPa, and 28.5 GPa, respectively. These values were higher than those of composites prepared via pressureless sintering and comparable to those of composites fabricated via hot pressing and/or using metal or oxide additives.     

Porosity control of porous silicon carbide ceramics

Porous SiC ceramics were fabricated by the carbothermal reduction of polysiloxane-derived SiOC containing polymer microbeads followed by sintering. The effect of the SiC powder:polysiloxane-derived SiC (SiC:PDSiC) ratio on the porosity and flexural strength of the porous SiC ceramics were investigated. The porosity generally increased with decreasing SiC:PDSiC ratio when sintered at the same temperature. It was possible to control the porosity of porous SiC ceramics within a range of 32–64% by adjusting the sintering temperature and SiC:PDSiC ratio while keeping the sacrificial template content to 50 vol%.The flexural strengths generally decreased with increasing porosity at the same SiC:PDSiC ratio. However, a SiC:PDSiC ratio of 9:1 and a sintering temperature of 1750 °C resulted in excellent strength of 57 MPa at 50% porosity. Judicious selection of the sintering temperature and SiC:PDSiC ratio is an efficient way of controlling the porosity and strength of porous SiC ceramics.     

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.     

Porous 2H-Silicon Carbide Ceramics Fabricated by Carbothermal Reaction between Silicon Nitride and Carbon

Porous SiC ceramics were synthesized by sintering pressed and pressed/CIPed powder compacts of α-Si₃N₄, carbon (Si₃N₄:C = 1:3 mol as ratio), and sintering aids, at 1600°C for few hours to achieve a reaction, and subsequently sintering at a temperature range of 1750°–1900°C, in an argon atmosphere. High porosities from 45%–65% were achieved by low shrinkage with large weight loss. Formation of pure 2H-SiC phase via a reaction between Si₃N₄ and carbon can be demonstrated by X-ray diffractometry. The resultant porous SiC samples were characterized by SiC grain microstructures, pore-size distribution, and flexural strength. This method has the advantage of fabricating high-porous SiC ceramics with fine microstructure and good properties at a relatively low temperature.     

The densification behavior,microstructure, mechanical,and thermionic emission properties of LaB6-SiC composite

The LaB₆-SiC composite with the different SiC content (0, 15, 30, 36, 50, 90, and 100 wt.%,) was densified by spark plasma sintering. The effects of SiC content on the densification behavior, microstructure, mechanical, and thermionic emission properties of LaB₆-SiC composite were systemically investigated. The results show that all the rapid shrinkage occurred at the heating stage during densification, and LaB₆-36 wt.%SiC composite owned the maximum shrinkage rate of 1.5 mm/min at T = 1798°C. The highest relative density of the composite decreased from 98.18% to 95.01% as the SiC content increased from 15 wt.% to 90 wt.%, under which the morphology of LaB₆ grain evaluated from the equiaxed to elongated structure, and LaB₆ grain size varied in the range of 5.05–11.42 μm. The similar eutectic structures were observed in the LaB₆-36 wt.% SiC composite because of some LaB₆ grains melting. Both the highest fracture toughness of 5.15 ± 0.56 MPa.m^1/2 and the highest bending strength of 313 ± 4.7 MPa belonged to the LaB₆-36 wt.% SiC composite, which also exhibited thermionic emission current density of 10.74 A/cm² and work function of 2.99 eV at T = 1873 K.     

Microstructural Control for Strengthening of Silicon Carbide Ceramics

Fine-grained (<1 μm) silicon carbide ceramics with high strength were obtained by using ultrafine (∼90 nm) β-SiC starting powders and a seeding technique for microstructural control. The microstructures of the as-hot-pressed and annealed ceramics without α-SiC seeds consisted of fine, uniform, and equiaxed grains. In contrast, the annealed material with seeds had a uniform, anisotropic microstructure consisting of elongated grains, owing to the overgrowth of β-phase on α-seeds. The strength, the Weibull modulus, and the fracture toughness of fine-grained SiC ceramics increased with increasing grain size up to ∼1 μm. Such results suggested that a small amount of grain growth in the fine grained region (<1 μm) was beneficial for mechanical properties. The flexural strength and the fracture toughness of the annealed seeded materials were 835 MPa and 4.3 MPa·m^1/2, respectively.     

Preparation of mullite ceramics with equiaxial grains from powders synthesized by the sol-gel method

Four different alumina content of mullite ceramics were fabricated by powders synthesized using the sol-gel method. The synthesis process of powders, microstructure evolution, mechanical and optical properties of the mullite ceramics were studied. The XRD results showed that the precursors transformed into aluminosilicate spinel phase at 1000 °C and mullite phase at 1200 °C. Equiaxial grains were easy to form in the alumina-rich mullite ceramics while elongated grains were easy to form in the alumina-poor mullite ceramics. With the increase of alumina content, the grain size of the samples firstly increased and then decreased, the number of elongated grains decreased while equiaxed grains increased. The flexural strength, compression strength, fracture toughness, and Vickers hardness all decreased firstly and then increased. While the infrared transmittance increased firstly and then decreased. The transmittance at 4 μm (thickness of 0.75 mm) of the ceramics containing 66mol% Al₂O₃ reached the highest (72%) when sintered at 1780 °C because of the equiaxial grains.     

Processing and properties of cordierite-silica bonded porous SiC ceramics

Cordierite-silica bonded porous SiC ceramics were fabricated by infiltrating a porous powder compact of SiC with cordierite sol followed by sintering at 1300–1400 °C in air. The porosity, average pore diameter and flexural strength of the ceramics varied 30–36 vol%, ~ 4–22 µm and ~ 13–38 MPa respectively with variation of sintering temperature and SiC particle sizes. In the final ceramics SiC particles were bonded by the oxidation-derived SiO₂ and sol-gel derived cordierite. The corrosion behaviour of sintered SiC ceramics was studied in acidic and alkaline medium. The porous SiC ceramics were observed to exhibit better corrosion resistance in acid solution.     

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.     

Mechanical and Thermal Properties of Pressureless Sintered Silicon Carbide Ceramics with Alumina–Yttria–Calcia

The effect of sintering temperature on the mechanical and thermal properties of SiC ceramics sintered with Al₂O₃–Y₂O₃–CaO without applied pressure was investigated. SiC ceramics containing A₂O₃–Y₂O₃–CaO as sintering additives can be sintered to >97% theoretical density at temperatures between 1750°C and 1900°C without applied pressure. A toughened microstructure, consisting of relatively large elongated grains and relatively small equiaxed grains, has been obtained when sintered at temperatures as low as 1800°C for 2 h in an argon atmosphere without applied pressure. The achievement of toughened microstructures under such mild conditions is the result of the additive composition. The thermal conductivity of the SiC ceramics increased with increasing sintering temperature because of the decrease in the lattice oxygen content of the SiC grains. Typical sintered density, flexural strength, fracture toughness, hardness, and thermal conductivity of the 1850°C‐sintered SiC, which consisted of 62.2% 4H, 35.7% 6H, and 2.1% 3C, were 99.0%, 628 MPa, 5.3 MPa·m^1/2, 29.1 GPa, and 80 W·(m·K)^?1, respectively.     

The effect of fabrication parameters on the mechanical properties of sintered reaction bonded porous Si3N4 ceramics

Porous silicon nitride ceramics were prepared via sintered reaction bonded silicon nitride at 1680 °C. The grain size of nitrided Si₃N₄ and diameter of post-sintered β-Si₃N₄ are controlled by size of raw Si. Porosity of 42.14–46.54% and flexural strength from 141 MPa to 165 MPa were obtained. During post-sintering with nano Y₂O₃ as sintering additive, nano Y₂O₃ can promote the formation of small β-Si₃N₄ nuclei, but the large amount of β-Si₃N₄ (>20%) after nitridation also works as nuclei site for precipitation, in consequence the growth of fine β-Si₃N₄ grains is restrained, the length is shortened, and the improvement on flexural strength is minimized. The effect of nano SiC on the refinement of the β-Si₃N₄ grains is notable because of the pinning effect, while the effect of nano C on the refinement of the β-Si₃N₄ grains is not remarkable due to the carbothermal reaction and increase in viscosity of the liquid phase.     

Pressureless sintered Al4SiC4 ceramics with Y2O3 addition

Highly densified Al₄SiC₄ ceramics with a relative density of 96.1% were prepared by pressureless sintering using 2 wt% Y₂O₃ as additives. The densification mechanism, phase composition, microstructures and mechanical properties of Al₄SiC₄ ceramics were investigated. Y₂O₃ in-situ reacted with the oxygen impurities in Al₄SiC₄ powder to form a yttrium aluminate liquid phase during sintering, which promoted the densification and anisotropic grain growth. The final Al₄SiC₄ ceramics were composed of equiaxed grains and columnar grains, and presented a bimodal grain distribution. The mechanical properties of the pressureless sintered Al₄SiC₄ ceramics were better than those reported for hot pressed Al₄SiC₄, including a flexural strength of 369 ± 24 MPa, fracture toughness of 4.8 ± 0.1 MPa m^1/2 and Vickers hardness of 11.3 ± 0.2 GPa. Pressureless sintering of Al₄SiC₄ ceramics is of great significance for the development and practical application of Al₄SiC₄ ceramic parts, especially with big size and complex shape.     

Porous Si3N4/SiC Ceramics Prepared via Nitridation of Si Powder with SiC Addition

Porous Si₃N₄/SiC ceramics with high porosity were prepared via nitridation of Si powder, using SiC as the second phase and Y₂O₃ as sintering additive. With increasing SiC addition, porous Si₃N₄/SiC ceramics showed high porosity, low flexural strength, and decreased grain size. However, the sample with 20wt% SiC addition showed highest flexural strength and lowest porosity. Porous Si₃N₄/SiC ceramics with a porosity of 36–45% and a flexural strength of 107‐46MPa were obtained. The linear shrinkage of all porous Si₃N₄/SiC ceramics is below 0.42%. This study reveals that the nitridation route is a promising way to prepare porous Si₃N₄/SiC ceramics with favorable flexural strength, high porosity, and low linear shrinkage.     

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.