Almost seamless joining of SiC using an in-situ reaction transition phase of Y3Si2C2

A new design of seamless joining was proposed to join SiC using electric field-assisted sintering technology. A 500 nm Y coating on SiC was used as the initial joining filler to obtain a desired transition phase of Y₃Si₂C₂ layer via the appropriate interface reactions with the SiC matrix. The phase transformation and decomposition of the transition phase of Y₃Si₂C₂ was designed to achieve almost seamless joining of SiC. The decomposition of the joining layer to SiC, followed up by the inter-diffusion and complete densification with the initial SiC matrix, resulted in the formation of an almost seamless joint at the temperature of 1900 °C. The bending strength of the seamless joint was 134.8 ± 2.1 MPa, which was comparable to the strength of the SiC matrix. The proposed design of seamless joining could potentially be applied for joining of SiC-based ceramic matrix composites with RE₃Si₂C₂ as the joining layer.     

Low temperature seamless joining of SiC using a Ytterbium film

Monolithic SiC, for the first time, was seamless joined at a low temperature of 1200 °C using electric field-assisted sintering technology. A 300 nm Yb coating on SiC was used as the joining filler to form Yb₃Si₂C₂ via an in-situ reaction with the SiC. A liquid phase was formed by an eutectic reaction between Yb₃Si₂C₂ and SiC. Almost completely seamless joints were formed by the precipitated SiC grains, which were fully consolidated with the SiC matrix with the help of in-situ formed liquid phase, followed by its elimination under the uniaxial pressure. The bending strength of the seamless joint joined at 1500 °C for 15 min was as high as 257.2 ± 31.1 MPa, which was comparable to the strength of the SiC matrix. As a result, the failure occurred in the matrix indicated a sound joint was obtained. The proposed low temperature seamless joining could potentially be used for joining of SiC-based composite.     

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.     

Fabrication and characterization of SPS sintered SiC-based ceramic from Y3Si2C2-coated SiC powders

The Y₃Si₂C₂ coating was in-situ synthesized on the surface of SiC powders to form SiC-Y₃Si₂C₂ core-shell structure by using a molten salt technique. Phase diagram calculations on Si-Y-C ternary phase at different temperatures well illustrated that the Y₃Si₂C₂ phase can be stable with SiC but will be in liquid state at 1560?°C. The liquid Y₃Si₂C₂ explained the enhanced consolidation of SiC ceramics and its disappearance after spark plasma sintering. Such Y₃Si₂C₂ coating could not only effectively improve the sintering, but also their mechanical and thermal properties of resultant ceramics. Typically, at 1700?°C, the bulk SiC ceramic presented a mean grain size of 2.5?um and relative density of 99.5% when the molar ratio of Y to SiC is 1:4 in molten salts; the Young’s modulus, indentation hardness and fracture toughness measured by indentation test were 451.7?GPa, 26.3?GPa and 7.9?M?Pam^1/2, respectively; the thermal conductivity is about 145.9?W/(m?K). Excellent thermal and mechanical properties could be associated with the fine grain size, optimized phase composition and improved grain boundary structure.     

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.     

Joining of SiC by Al infiltrated TiC tape: Effect of joining parameters on the microstructure and mechanical properties

SiC ceramics were successfully joined by Al infiltrated TiC tapes at 900-1100 °C for 0.5-2 h in vacuum. Phase constituents, microstructure and mechanical strength of the prepared SiC joints were characterized. The prepared SiC joints display dense interlayer and crack-free interface. The interlayer primarily consists of TiC and Al phases, together with small amount of TiAl₃ and trace of Al₄C₃. With increasing the joining temperature or time, the interface layer either thickens or grows to multiple layers. The bending strengths of the SiC joints are higher than 190 MPa as bonded at present conditions, and are closely related with the property of interface and interlayer.     

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.     

Thickness-dependent phase evolution and bonding strength of SiC ceramics joints with active Ti interlayer

A robust solid state diffusion joining technique for SiC ceramics was designed with a thickness-controlled Ti interlayer formed by physical vapor deposition and joined by electric field-assisted sintering technology. The interface reaction and phase revolution process were investigated in terms of the equilibrium phase diagram and the concentration-dependent potential diagram of the Ti-Si-C ternary system. Interestingly, under the same joining conditions (fixed temperature and annealing duration), the thickness of the Ti interlayer determined the concentration and distribution of the Si and C reactants in the resulting joint layer, and the respective diffusion distance of Si and C into the Ti interlayer differentiated dramatically during the short joining process (only 5 min). In the case of a 100 nm Ti coating as an interlayer, the C concentration in the joint layer was saturated quickly, which benefited the formation of a TiC phase and subsequent Ti₃SiC₂ phase. The SiC ceramics were successfully joined at a low temperature of 1000 °C with a flexural strength of 168.2 MPa, which satisfies applications in corrosive environments. When the Ti thickness was increased to 1 μm, Si atoms diffused easily through the diluted Ti-C alloy (a dense TiC phase was not formed), and the Ti₅Si₃ brittle phase formed preferentially. These findings highlight the importance of the diffusion kinetics of the reactants on the final composition in the solid state reaction, particularly in the joining technique for covalent SiC ceramics.     

Joining of Cf/SiC composites and Si3N4 ceramic with Y2O3–Al2O3–SiO2 glass filler for high-temperature applications

C_f/SiC composites and Si₃N₄ ceramics are candidate materials for applications in thermal protection system. This paper investigated the joining of C_f/SiC and Si₃N₄ using Y₂O₃–Al₂O₃–SiO₂ glass. The reliability of joints was evaluated by thermal shock tests. In this present work, the typical joint structure was C_f/SiC-glass-Si₃N₄. The results demonstrate that Direct bonding has been identified as the interfacial bonding mechanism at the SiC/glass and glass/Si₃N₄ interfaces. The maximum shear strength of the C_f/SiC–Si₃N₄ joint was ~34 MPa, which delivered an effective method to achieve strong, reliable bonding between the dissimilar materials. In addition, after thermal shock for 10 cycles, the residual strength remained ~13 MPa. Bubbles instead of microcracks formed in the glass filler, which was the main factor causing the degradation of the joint performance. It is suggested that improving the high temperature resistance of joining materials is the key to realize the application of this joint structure.     

Wetting of SiC by Al-Ti alloys and joining by in-situ formation of interfacial Ti3Si(Al)C2

Two pressureless and reliable procedures for brazing SiC-based materials have been designed. The joining was obtained by the in-situ formation of a Ti₃Si(Al)C₂ MAX phase using simple Al-Ti interlayers. Wettability studies were conducted using several Al-Ti alloys in contact with SiC at 1500?°C. The interfacial microstructures and thermodynamic analysis demonstrated that liquid Al₃Ti in contact with SiC formed a well-bonded Ti₃Si(Al)C₂ interfacial layer. These findings guided the design of two joining methods: one consisted of the simple infiltration of Al₃Ti into the brazing seam, while an Al₃Ti paste/Ti/Al₃Ti paste interlayer assembly was designed for the second process. Sound interfaces without cracks were obtained in both processes. The average shear strength was very high, 296?MPa, for the infiltration method; the drawback was the presence of residual Al. Joining through Al₃Ti/Ti/Al₃Ti interlayers avoided the presence of low-temperature melting phases, with lower shear strength: 85 or 89?MPa depending on the testing method.     

Preparation of crystalline ytterbium disilicate environmental barrier coatings using suspension plasma spray

In high-speed modern industries, high-temperature stability of materials is essential. A promising high-temperature material currently attracting attention is silicon carbide (SiC)-based ceramic matrix composites (CMC). However, a disadvantage of these materials is their reduced lifetime in an oxidizing atmosphere. To overcome this, environmental barrier coating can be employed. In this study, we aimed to fabricate an environmental barrier coating using suspension plasma spray with Yb₂Si₂O₇, which exhibits excellent oxidation resistance and a similar thermal expansion coefficient to SiC. To prepare the crystalline Yb₂Si₂O₇ coating layer, the gas concentration of the plasma spray was adjusted, and then the suspension manufacturing solvent was adjusted and sprayed. The prepared coating samples were analyzed by X-ray diffraction, scanning electron microscope, transmission electron microscopes, and energy dispersive X-ray spectroscopy to determine phase and microstructure changes. Highly crystalline ytterbium disilicate was observed at low plasma enthalpy with no hydrogen and 20% addition of water.     

In-situ synthesis of ternary layered Y3Si2C2 ceramic on silicon carbide fiber for enhanced electromagnetic wave absorption

A novel ternary layered ceramic of Y₃Si₂C₂ was successfully in-situ synthesized on the surface of home-made third-generation KD-SA SiC fiber for the first time by molten salt method aimed at improving the electromagnetic wave (EMW) absorption. After in-situ synthesis of Y₃Si₂C₂ ceramic layer on SiC fiber (SiC_f/Y₃Si₂C₂), significantly improved EMW absorption performance was obtained. The minimum reflection loss (RL_min) of ?16.97 dB was reached in SiC_f/Y₃Si₂C₂ composites at the thickness of only 2.19 mm, and the effective absorption bandwidth (EAB) was up to 5.44 GHz (12.56–18 GHz) at a thin thickness of 2.64 mm. The improvement in EMW absorption of SiC_f/Y₃Si₂C₂ is mainly attributed to enhanced dielectric loss and conduction loss resulting from increased heterogeneous interfaces and multiple reflections and scattering originating from net structure. The SiC_f/Y₃Si₂C₂ could be a promising EMW absorber for application in high-performance EMW absorbing materials.     

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.     

Synthesis of Ti3SiC2 coatings onto SiC monoliths from molten salts

Coatings with composition close to Ti₃SiC₂ were obtained on SiC substrates from Ti and Si powders with the molten NaCl method. In this work, the growth of coatings by reaction in the salt between monolithic SiC substrates and titanium powder is obtained between 1000 and 1200 °C. At 1000 °C, a coating of 8 µm thickness is formed in 10 h whereas a thin coating of 0.5 µm has been grown in 2 h. A lack in silicon was first found in the coatings prepared at 1100 and 1200 °C. For these temperatures, the addition of silicon powder in the melt had a favorable effect on the final composition, which is found very close to the composition of Ti₃SiC₂. The reaction mechanism implies the formation of TiC_x layers in direct contact with the SiC substrate and the presence of more or less important quantities of Ti₃SiC₂ and Ti₅Si₃C_x in the upper layers.     

Fabrication and characterisation of single-phase Hf2Al4C5 ceramics

Single-phase Hf₂Al₄C₅ ternary carbide was fabricated from Hf/Al/C powder mixtures by pressure assisted sintering techniques such as hot pressing and spark plasma sintering at 1900 °C for 3 h and 10 min, respectively. XRD confirmed that the ternary carbide started to form at temperatures as low as 1500 °C and with total formation of Hf₂Al₄C₅ after reactive sintering for 1 h at 1900 °C. It is evident from HRTEM that two Hf-C layers were sandwiched with 4 Al-C layers (Al₄C₃) in the Hf₂Al₄C₅ ternary carbide. Tight interlocking of grains, faceted grains and stacking faults were occasionally observed. Thermal conductivity of Hf₂Al₄C₅ is measured to be 14 w m^?1k^?1 from room temperature to 1300 °C. The oxidation studies carried out at 1300 °C for 3 h reveal that the oxidation layer thickness is around 220 μm and it contains microcracks closer to sample surface whereas the interface looks seamless without any cracking or spallation of the oxide layer.     

Investigation of MoSi2 melt infiltrated RSiC and its oxidation behavior

Melt infiltration process was employed to fill molten MoSi₂ into the pores of recrystallized silicon carbide (RSiC) to improve the oxidation resistance of RSiC, and an almost fully dense RSiC-MoSi₂ composite with the microstructure of two-phase interpenetrated network was obtained. The phase compositions of the composites are mainly SiC and MoSi₂, including a small amount of Mo_4.8Si₃C_0.6 and Mo₅Si₃. The flexural strength of the composites at room temperature was 11-32% higher than that of as-received RSiC. The cyclic oxidation tests at 1500 °C indicated that both the RSiC-MoSi₂ composites and RSiC exhibited a parabolic oxidation behavior, and the corresponding parabolic rate constants of the composites were almost an order of magnitude lower than those of RSiC, resulting in a great improvement of oxidation resistance of RSiC-MoSi₂.     

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.     

Microstructural evolution and characterization of interfacial phases in diffusion-bonded SiC/Ta–5W/SiC joints

The evolution of reaction phases formed in diffusion-bonded SiC/Ta–5W/SiC joints was investigated at a joining temperature of 1500–1700 °C for 10–90 min. The effects of bonding temperature and holding time on the phase evolution were found to be directly correlated with the thickness of the interfacial reaction layer when a 100-μm-thick Ta–5W interlayer was used for joining. In the case of a ~7-μm-thick reaction layer, the interfacial phase constitution consisted of a layered SiC/(Ta,W)C/(Ta,W)₅Si₃/(Ta,W)₂Si/(Ta,W)_xSi_y/Ta–5W structure. In the reaction layer with a thickness of ~11–26 μm, the interfacial structure evolved into SiC/(Ta,W)C/(Ta,W)₅Si₃/(Ta,W)C/(Ta,W)_xSi_y/(Ta,W)₂Si/(Ta,W)_xSi_y/Ta–5W, in which an additional (Ta,W)C/(Ta,W)_xSi_y layer was inserted between (Ta,W)₅Si₃ and (Ta,W)_xSi_y owing to the precipitation of carbon from the (Ta,W)₅Si₃ layer. When the Ta–5W interlayer was fully consumed to form a stable reaction product, namely the equilibrium state, (Ta,W)_xSi_y and (Ta,W)₂Si were eventually transformed into (Ta,W)₅Si₃, and the final interface structure that was obtained was SiC/(Ta,W)C/(Ta,W)₅Si₃/(Ta,W)C/(Ta,W)₅Si₃/(Ta,W)C. This achievement will benefit the design, control, and characterization of SiC/metal interfaces.