Low-temperature joining of SiC ceramics by NITE phase using CaO-Al2O3-MgO-SiO2 glass as an additive combined with surface oxidation

Low-temperature joining of SiC ceramics using raw CaO-Al₂O₃-MgO-SiO₂ mixed powders (CAMS-P) and CaO-Al₂O₃-MgO-SiO₂ glass (CAMS-G) as additives for the liquid-phase sintering of SiC nanopowders (NITE phase) in combination with surface oxidation was studied. Using CAMS-P as an additive for SiC joining required 1650 °C and produced a lower shear strength of 77.2 ± 3.5 MPa, compared to untreated SiC (108.2 ± 15.8 MPa). Using CAMS-G as an additive, the compactness of SiC joints obtained at 1550 °C was higher than that of NITE joints obtained at 1650 °C with CAMS-P as an additive. Nonetheless, the low joining temperature resulted in gaps and delaminations at the interface, and the joints strength was only 48.3 ± 5.6 MPa. Incorporating CAMS-G as an additive and surface oxidation achieved reliable NITE phase joining at 1550 °C, with no observed gaps or delaminations at the interface. The resulting joints strength was as high as 100.0 ± 0.8 MPa. The joining mechanism was discussed and compared, involving microstructural analysis.     

Mechanical properties of silicon carbide—in situ zirconium carbonitride composites

SiC–Zr₂CN composites were fabricated by conventional hot pressing from β-SiC and ZrN powders with 2 vol% equimolar Y₂O₃–Sc₂O₃ as a sintering additive. The effects of the ZrN addition on the room-temperature (RT) mechanical properties and high-temperature flexural strength of the SiC–Zr₂CN composites were investigated. The fracture toughness gradually increased from 4.2 ± 0.3 MPa·m^1/2 for monolithic SiC to 6.3 ± 0.2 MPa·m^1/2 for a SiC–20 vol% ZrN composite, whereas the RT flexural strength (546 ± 32 MPa for the monolithic SiC) reached its maximum of 644 ± 87 MPa for the SiC–10 vol% ZrN composite. The monolithic SiC had improved strength at 1200°C, whereas the SiC–Zr₂CN composites could not retain their RT strengths at 1200°C. The typical flexural strength values of the SiC–0, 10, and 20 vol% ZrN composites at 1200°C were 650 ± 53, 448 ± 31, and 386 ± 19 MPa, whereas their RT strength values were 546 ± 32, 644 ± 87, and 528 ± 117 MPa, respectively.     

Low-temperature joining of SiC ceramics using NITE phase with Al2O3-Ho2O3 additive

In order to avoid the property degradation resulting from high-temperature joining process, nano-infiltrated transient eutectoid (NITE) phase with the Al₂O₃-Ho₂O₃ as the joining adhesives was adopted to join silicon carbide (SiC) ceramics with the attempts to lower down the joining temperature. The liquid-phase-sintered silicon carbide (LPS-SiC) specimens were joined at 1500-1800°C by spark plasma sintering (SPS) under the pressure of 20 MPa. The results of the shear test and microstructure observation showed that the joining process could be finished at a relatively lower temperature (1700°C) compared to other NITE-phase joining. In contrast to the shear strength of 186.4 MPa derived from the SiC substrate, the joint exhibited the shear strength of 157.8 MPa with the fully densified interlayer.     

Joining of silicon carbide ceramics using a silicon carbide tape

This paper reports the joining of liquid-phase sintered SiC ceramics using a thin SiC tape with the same composition as base SiC material. The base SiC ceramics were fabricated by hot pressing of submicron SiC powders with 4 wt% Al₂O₃–Y₂O₃–MgO additives. The base SiC ceramics were joined by hot-pressing at 1800-1900°C under a pressure of 10 or 20 MPa in an argon atmosphere. The effects of sintering temperature and pressure were examined carefully in terms of microstructure and strength of the joined samples. The flexural strength of the SiC ceramic which was joined at 1850°C under 20 MPa, was 343 ± 53 MPa, higher than the SiC material (289 ± 53 MPa). The joined SiC ceramics showed no residual stress built up near the joining layer, which was evidenced by indentation cracks with almost the same lengths in four directions.     

The influence of different SiC amounts on the microstructure,densification, and mechanical properties of hot-pressed Al2O3-SiC composites

The hot pressing process of monolithic Al₂O₃ and Al₂O₃-SiC composites with 0-25 wt% of submicrometer silicon carbide was done in this paper. The presence of SiC particles prohibited the grain growth of the Al₂O₃ matrix during sintering at the temperatures of 1450°C and 1550°C for 1 h and under the pressure of 30 MPa in vacuum. The effect of SiC reinforcement on the mechanical properties of composite specimens like fracture toughness, flexural strength, and hardness was discussed. The results showed that the maximum values of fracture toughness (5.9 ± 0.5 MPa.m^1/2) and hardness (20.8 ± 0.4 GPa) were obtained for the Al₂O₃-5 wt% SiC composite specimens. The significant improvement in fracture toughness of composite specimens in comparison with the monolithic alumina (3.1 ± 0.4 MPa.m^1/2) could be attributed to crack deflection as one of the toughening mechanisms with regard to the presence of SiC particles. In addition, the flexural strength was improved by increasing SiC value up to 25 wt% and reached 395 ± 1.4 MPa. The scanning electron microscopy (SEM) observations verified that the increasing of flexural strength was related to the fine-grained microstructure.     

Joining of SiC ceramics by combining NITE-SiC interlayer and its thickness control

Combined with the thickness control of interlayers (∼10 µm and ∼60 µm), SiC nano-powders with Al₂O₃-Y₂O₃-MgO-CaO additive (NITE-SiC) were used as the joining materials to achieve the low-temperature joining of SiC ceramics. Some residual pores were observed in the interlayer with a thickness of ∼60 µm after joining at 1650 ℃, and the shear strength of SiC joints measured was 39.3 ± 5.5 MPa. Observations showed the fracture of joints occurred at the interlayer. When the thickness of the interlayer decreased to ∼10 µm, no cracks or porosity were observed at the interface region after joining at 1650 ℃. The shear strength of SiC joints increased to 69.5 ± 8.9 MPa, and the fracture originated from the matrix. The results demonstrated using NITE-SiC with Al₂O₃-Y₂O₃-MgO-CaO additive as the joining layer and reducing the thickness of the interlayer could lower the joining temperature and significantly improve the mechanical strength of joints.     

Residual thermal stress of SiC/Ti3SiC2/SiC joints calculation and relaxed by postannealing

Residual thermal stresses in SiC/Ti₃SiC₂/SiC joining couples were calculated by Raman spectra and simulated by finite element analysis, and then relaxed successfully by postannealing. The results showed that the thermal residual stress between Ti₃SiC₂ and SiC was about on the order of 1 GPa when cooling from 1300°C to 25°C. The thermal residual stresses can be relaxed by the recovery of structure disorders during postannealing. When the SiC/Ti₃SiC₂/SiC joints postannealed at 900°C, the bending strength reached 156.9 ± 13.5 MPa, which was almost twice of the as‐obtained SiC/Ti₃SiC₂/SiC joints. Furthermore, the failure occurred at the SiC matrix suggested that both the flexural strength of joining layer and interface were higher than the SiC matrix.     

Microstructure and mechanical properties of SiC-SiC joints joined by spark plasma sintering

The development of reliable joining technology is of great importance for the full use of SiC. Ti₃SiC₂, which is used as a filler material for SiC joining, can meet the demands of neutron environment applications and can alleviate residual stress during the joining process. In this work, SiC was joined using different powders (Ti₃SiC₂ and 3Ti/1.2Si/2C/0.2Al) as filler materials and spark plasma sintering (SPS). The influence of the joining temperature on the flexural strength of the SiC joints at room temperature and at high temperatures was investigated. Based on X-ray diffraction and scanning electron microscopy analyses, SiC joints with 3Ti/1.2Si/2C/0.2Al powder as the filler material possess high flexural strengths of 133 MPa and 119 MPa at room temperature and at 1200 °C, respectively. The superior flexural strength of the SiC joint at 1200 °C is attributed to the phase transformation of TiO₂ from anatase to rutile.     

Low-temperature joining of SiC ceramics with Y2O3-Al2O3 interlayer by SiO2-based liquid phase extrusion strategy

In order to reduce the joining temperature of SiC ceramics by glass-ceramic joining, some oxides were usually introduced into to Y₂O₃–Al₂O₃ for reducing the eutectic temperature. However, the joints might have poor high-temperature resistance due to the low melting point of the joining layer. In the present work, based on novel SiO₂-based liquid phase extrusion strategy, joining of SiC ceramics with Y₂O₃–Al₂O₃ interlayer was carried out by using Y₂O₃–Al₂O₃–SiO₂ as the filler through spark plasma sintering (SPS). The SiO₂-free interlayer of Y₂O₃–Al₂O₃ was used for comparison. It was found that SiC joints using Y₂O₃–Al₂O₃ could be only joined at a high temperature of 1800 °C, and the thickness of the interlayer was about 20 μm. The shear strength of the joint obtained at 1800 °C was 89.62 ± 4.67 MPa and the failure located in the SiC matrix. By contrast, reliable joining of SiC ceramics could be finished at as low as 1550 °C by extrusion of SiO₂-containing liquid phase when using Y₂O₃–Al₂O₃–SiO₂ as the interlayer, alongside the interlayer thickness of only several microns. The joint strengths after joining at 1550 °C was 84.90 ± 3.48 MPa and the failure located in matrix position. The joining mechanism was discussed by combining the detailed microstructure analysis and phase diagram.     

High-strength SiC joints fabricated at a low-temperature of 1400°C using a novel low activation filler of Praseodymium

High-strength SiC joints were successfully obtained by electric current field-assisted sintering technique at a low temperature of 1400°C using a Pr coating (100 nm) as the initial joining filler. A Pr₃Si₂C₂ transient phase was formed in situ by the interfacial reaction, while the eutectic reaction between Pr₃Si₂C₂ and SiC at ∼1150°C resulted in the formation of a liquid phase. The liquid phase promoted the atomic diffusion at the interface and improved consolidation of the newly precipitated nano-sized SiC with the SiC matrix. This led to the formation of partially seamless joints of SiC. When the thickness of the joining layer decreased from 1 to 100 nm, the content of the residual Pr-O phase at the interface decreased, while the bending strength of the joints increased. A sound SiC joint with a bending strength of 227 ± 12 MPa was obtained at such a low temperature as 1400°C when a 100 nm Pr coating was applied.     

Harmonized toughening and strengthening in pressurelessly reactive-sintered Ta0.8Hf0.2C-SiC composite

Ta_0.8Hf_0.2C-27?vol%SiC (99.0% in relative density) composite was toughened and strengthened via pressurelessly in-situ reactive sintering process. HfC and β-SiC particles were formed after reaction of HfSi₂ and carbon black at 1650?°C. Ta_0.8Hf_0.2C was obtained from solid solutioning of HfC and commercial TaC. The β-α phase transformation of SiC proceeded below 2200?°C. High aspect ratio, platelet-like α-SiC grains formed and interconnected as interlocking structures. Toughness and flexural strength values of 5.4?±?1.2?MPa?m^1/2 and 443?±?22?MPa were measured respectively. The toughening mechanisms by highly directional growth of discontinuous α-SiC grains were crack branching, bridging and deflection behaviors.     

Fabrication and characterization of cordierite-bonded porous SiC ceramics

A reaction bonding technique was used for the preparation of cordierite-bonded porous SiC ceramics in air from α-SiC, α-Al₂O₃ and MgO, using graphite as the pore-forming agent. Graphite was burned out to produce pores and the surface of SiC was oxidized to SiO₂ at high temperature. With further increasing the temperature, SiO₂ reacted with α-Al₂O₃ and MgO to form cordierite. SiC particles were bonded by the cordierite and oxidation-derived SiO₂. The reaction bonding characteristics, phase composition, open porosity, pore size distribution and mechanical strength as well as microstructure of porous SiC ceramics were investigated. The pore size and porosity were strongly dependent, respectively, on graphite particle size and volume fraction. The porous SiC ceramics sintered at 1350 °C for 2 h exhibited excellent combination properties, the flexural strength of 26.0 MPa was achieved at an open porosity of 44.51%.     

High strength and high light transmittance sapphire/sapphire joints bonded using a La2O3-Al2O3-SiO2 glass filler

A novel La₂O₃-Al₂O₃-SiO₂ (LAS) glass was used as filler to join transparent sapphire for obtaining high strength and high light transmittance joints. The results show that the LAS glass filler had compatible coefficient of thermal expansion (CTE) with sapphire and excellent wetting ability on sapphire. During the joining process, no interfacial reaction occurred and the brazing seams were in a completely amorphous state under fast cooling conditions (~50 °C/min). With increased joining temperature, the mutual dissolution and diffusion between sapphire and the LAS filler were enhanced. The flexural strength of joints first increased and then decreased with an increase in the joining temperature from 1400 °C to 1550 °C. The optimal flexural strength of joint reached 325 MPa, which almost was the same as the strength of sapphire substrate. At 500 nm, the in-line transmittance of this joint was 80.5%, which was close to that of sapphire (84.2%).     

Pressureless joining of SiC ceramics with magnesia-alumina-silica glass ceramics

Liquid phase sintered SiC ceramics were joined using magnesia-alumina-silica (MAS) glass-ceramic fillers without applied pressure. Four different filler compositions with 9.3–25.2 wt.% MgO, 20.7–33.6 wt.% Al₂O₃, and 49.2–68.1 wt.% SiO₂ were studied. The effects of filler composition and joining temperature (1450–1600°C) on the joint strength were investigated. All compositions exhibited an optimum joining temperature at which the maximum joint strength was obtained. A low joining temperature resulted in poor wetting of the SiC substrate due to the high viscosity of the filler. Whereas a high joining temperature caused dewetting and large unfilled sections in the interlayer due to the deleterious interfacial reactions. The joint strength was inversely proportional to the interlayer thickness, which was a function of filler composition and joining temperature. The SiC ceramic joined at 1525°C with MgO-25 wt.% Al₂O₃-60 wt.% SiO₂ filler exhibited a four-point bending strength of 286 ± 40 MPa.     

Preparation and properties of porous SiC–Al2O3 ceramics using coal ash

In this paper, we first reported that porous SiC–Al₂O₃ ceramics were prepared from solid waste coal ash, activated carbon, and commercial SiC powder by a carbothermal reduction reaction (CRR) method under Ar atmosphere. The effects of addition amounts of SiC (0, 10, 15, and 20 wt%) on the postsintering properties of as-prepared porous SiC–Al₂O₃ ceramics, such as phase composition, microstructure, apparent porosity, bulk density, pore size distribution, compressive strength, thermal shock resistance, and thermal diffusivity have been investigated. It was found that the final products are β-SiC and α-Al₂O₃. Meanwhile, the SEM shows the pores distribute uniformly and the body gradually contacts closely in the porous SiC–Al₂O₃ ceramics. The properties of as-prepared porous SiC–Al₂O₃ ceramics were found to be remarkably improved by adding proper amounts of SiC (10, 15, and 20 wt%). However, further increasing the amount of SiC leads to a decrease in thermal shock resistance and mechanical properties. Porous SiC–Al₂O₃ ceramics doped with 10 wt% SiC and sintered at 1600°C for 5 hours with the median pore diameter of 4.24 μm, room-temperature compressive strength of 21.70 MPa, apparent porosity of 48%, and thermal diffusivity of 0.0194 cm²/s were successfully obtained.     

Ultrafast low-temperature near-seamless joining of Cf/SiC using a sacrificial Pr3Si2C2 filler via electric current field-assisted sintering technique

A novel layered structure material, Pr₃Si₂C₂, was synthesized at a low temperature of 850 °C using a molten salt approach for the first time, and subsequently used as the joining filler for carbon fibers reinforced SiC composites (C_f/SiC). A robust near-seamless C_f/SiC joint was successfully obtained at 1509 °C (T_i) for 30 s, while an ultrafast heating rate of 6000 °C/min was applied via electric field-assisted sintering technology. The near-seamless joining process was attributed to the newly precipitated SiC grains, which were densified well with the C_f/SiC matrix by liquid-assisted sintering. The liquid phase was in-situ formed by the eutectic reaction between Pr₃Si₂C₂ and SiC. The shear strength of the near-seamless joint obtained at 1509 °C for 30 s was 17.6 ± 3.0 MPa. The failure occurred in the C_f/SiC matrix. The formation of near-seamless C_f/SiC joints dismisses the issues related to thermal mismatch between C_f/SiC matrices and traditional joining fillers.     

High temperature strength of silicon carbide sintered with 1 wt.% aluminum nitride and lutetium oxide

A heat-resistant SiC ceramic was developed from submicron β-SiC powders using a small amount (1 wt.%) of AlN–Lu₂O₃ additives at a molar ratio of 60:40. Observation of the ceramic using high-resolution transmission electron microscopy (HRTEM) showed a lack of amorphous films in both homophase (SiC–SiC) boundaries and junction areas. The junction phase consisted of Lu–Si–O elements, and the homophase boundaries contained Lu, Al, O, and N atoms as segregates. The ceramic maintained its room temperature (RT) strength up to 1600 °C. The flexural strength of the ceramic was 630 MPa and 633 MPa at RT and 1600 °C, respectively.     

Direct bonding of silicon carbide ceramics sintered with yttria

SiC ceramics sintered with yttria were successfully joined without an interlayer by conventional hot pressing at lower temperatures (2000–2050 °C) compared to those of the sintering temperatures (2050–2200 °C). The joined SiC ceramics sintered with 2000 ppm Y₂O₃ showed almost the same thermal conductivity (˜198 Wm⁻¹ K⁻¹), fracture toughness (3.7 ± 0.2 MPa m^1/2), and hardness (23.4 ± 0.8 GPa) as those of the base material, as well as excellent flexural strength (449 MPa). In contrast, the joined SiC ceramics sintered with 4 wt% Y₂O₃ showed very high thermal conductivity (˜204 Wm⁻¹ K⁻¹) and excellent flexural strength (˜505 MPa). Approximately 16–22% decreases in strength compared to those of the base SC materials were observed in both joined ceramics, due to the segregation of liquid phase at the interface. This issue might be overcome by preparing well-polished and highly flat surfaces before joining.     

Joining of β-SiC by spark plasma sintering

Spark plasma sintering (SPS) was employed to join monolithic β-SiC with or without titanium as intermediate joining material. Both the localized and rapid heating contributed to the inherent energy saving of electric current assisted joining technique. The effects of uniaxial pressure and surface preparation were analyzed independently with respect to the flexural strength and the morphology of the joints. In particular samples polished down to 1 μm and joined at 1900 °C for 5 min achieved the strength of the as received material. The failure occurred outside the joining interface, confirming the optimum quality of the joint. Pressure in combination with surface preparation was necessary to achieve perfect adhesion and pore free direct joining of SiC. The use of Ti foil as a joining material and pressure allowed joining of unpolished SiC.     

Reactive consolidation and high-temperature strength of HfB2–SiB6

During the spark plasma sintering at 1900 °C, SiB₆ decomposes into cubic silicon carbide and boron carbide, owing to the reducing environment of the furnace. For the HfB₂-SiB₆ ceramic improvement in hardness (24.5 ± 0.7 GPa) was attributed to the formation of the B₁₂(C,Si,B)₃. Fracture toughness by indentation (6.8 ± 2.4 MPa·m^1/2), single-edge notched bend specimens (4.6 ± 0.4 MPa·m^1/2) and room-temperature strength (513 ± 21 MPa) of the HfB₂–SiB₆ composite produced by spark plasma sintering was higher or on the same level as the HfB₂–SiC ceramics. The high-temperature flexural strength tests suggested that the strength would decrease monotonically with an increase in temperature. At or below 1600 °C, only a linear stress-strain response was observed, and resulted into a mean strength of ~320 MPa. During the tests at 1800 °C, we observed a nonlinear deformation indicating ongoing plastic deformation which led to a strength decrease down to 230 ± 30 MPa.