Effect of Zr addition on the interfacial reaction of the SiC joint brazed by Inconel 625 powder filler

Ni-based alloys are believed to be the most suitable brazing fillers for SiC ceramic application in a nuclear environment. However, graphite, which severely deteriorates the mechanical property of the joint, is inevitable when Ni reacts with SiC. In this paper, Different amounts of Zr powders are mixed with Inconel 625 powders to braze SiC at 1400 °C. When Zr addition reaches 40 wt%, the brazed seam confirms the absence of graphite. This research proves that Zr can avoid the graphite’s formation by suppressing Ni’s activity. The room-temperature shear strength of the joint with graphite’s absence is tested to be 81.97 MPa, which is almost three times higher than that of the joint with graphite. The interfacial reaction process and mechanism of the SiC joint are investigated and explained in this paper using thermodynamic calculations.     

Joining of SiC ceramics using the Ni-Mo filler alloy for heat exchanger applications

In order to meet the sealing demands of SiC heat exchanger, the Ni-Mo filler alloy was designed, prepared and employed to braze SiC ceramics. Wetting behavior of the Ni-Mo filler alloy on SiC ceramics and interfacial microstructure of the brazed joints were systematically characterized using optical observation furnace and XRD, SEM, EDS, TEM, respectively. Flexural strengths of the brazed joints at room temperature and high temperature were measured with four-point flexural strength method. HCl immersion test was performed to evaluate the corrosion resistance of the joints. The Ni-Mo filler alloy exhibited excellent wettability on SiC ceramics. During the process of brazing, SiC reacted with element Ni of the Ni-Mo filler alloy, resulting in the formation of Ni₂Si + graphite reaction layer adjacent to the SiC substrate. Ni₃Mo₃C and Ni₂Si compounds were precipitated at the center of brazing seam. When the brazing temperature increased from 1250 ℃ to 1400 ℃, the thickness of Ni₂Si + graphite layer increased gradually. The maximum room-temperature flexural strength of 174 ± 33 MPa was obtained when brazed at 1300 ℃ for 40 min. The joints also exhibited stable high-temperature strength and acid corrosion resistance. When the test temperature was 700 ℃, 800 ℃, 900 ℃, the joints gave the strength retention rate of 92.5 %, 79.8 %, 67.2 %, respectively. It was believed that the formation of high melting point phases played an important role. Residual strength of the joints after HCl corrosion exceeded 130 MPa, revealing a good potential for applications in corrosion environment.     

Interfacial reaction mechanism of SiC joints joined by pure nickel foil

To investigate the reaction mechanism of Ni/SiC system, 0.1 μm-thick pure nickel foil is used to join SiC ceramic at 1245 °C for different times. Interfacial melting is calculated to occur at 964 °C along the interface due to the low eutectic point of θ-Ni₂Si and NiSi, a periodical layered structure, consisting alternating layers of silicides/silicides+graphite, is formed along the interface due to periodical detachment of graphite from SiC reaction interface during the reactions between Ni-Si liquid phase and SiC. The reaction products of Ni/SiC are successfully predicted by CALPHAD method, based on a home-made Ni-Si-C ternary database. The reaction processes between Ni and SiC and the morphology changes of the joined seam are discussed in detail in this paper. The average shear strengths of SiC joints held for 15 min, 30 min and 60 min are tested to be 16.53 MPa, 19.32 MPa and 29.43 MPa, respectively.     

Effect of Ti addition on the wetting and brazing of Sn0.3Ag0.7Cu filler on SiC ceramic

The wetting behavior of Sn0.3Ag0.7Cu (SAC) filler with the addition of Ti on SiC ceramic was investigated using sessile drop method. SiC/SiC was brazed by SAC-Ti filler with different Ti content at 1223 K (950°C) for 10 minutes. The wettability of SAC-Ti filler on SiC was significantly enhanced with the addition of Ti. The contact angle decreased at first and then increased with increasing Ti content. The lowest contact angle of 9° was obtained with SAC-1.5Ti (wt%) filler. When Ti content further increased to 2.0 wt%, the contact angle increased, due to the intense reaction of Ti–Sn. The reaction between Ti and SiC controlled the wetting behavior of SAC-Ti on the SiC substrate and the reaction products such as TiC and Ti₅Si₃ were formed. The wetting of SAC-Ti on SiC was reaction-controlled. Interfacial reaction products TiC and Ti₅Si₃ were observed. The wetting activation energy in spreading stage was calculated to be 129.3 kJ/mol. Completely filled SiC/SiC joints were obtained using the filler with Ti content higher than 0.5 wt%. The fillet height increased firstly then decreased with mounting Ti content. The shear strength of joints increased first with the addition of Ti then decreased with Ti content increasing to 2.0 wt%. The highest shear strength of 35.7 MPa was obtained with SAC-1.5 Ti (wt%) filler.     

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.     

Joining of Cf/SiC composite to Ti-6Al-4V with (Ti-Zr-Cu-Ni)+Ti filler based on in-situ alloying concept

In this paper, a novel brazing process based on in-situ alloying concept was carried out to join C_f/SiC composite to TC4 alloy at 940 °C for 20 min. Mixed powders of Ti-Zr-Cu-Ni alloy and pure Ti metal were used as interlayer. In the process, Ti-Zr-Cu-Ni alloy melted and then dissolved pure Ti metal via liquid-solid reactions, achieving in-situ alloying of the interlayer. The interfacial microstructure and formation mechanism of the brazed joints were investigated. The effect of Ti powder content on the microstructure and the mechanical properties of joints were analyzed. The results showed that: the maximum lap-shear strength of the in-situ alloying brazed joints was 283±11 MPa when using (Ti-Zr-Cu-Ni)+40 vol% Ti composite filler, and this value was 79% higher than the mechanical strength when using Ti-Zr-Cu-Ni alone. A reaction layer of (Ti,Zr)C+Ti₅Si₃ formed near C_f/SiC composite side, while a diffusion layer of Ti₂Cu+Ti(s,s) formed near Ti-6Al-4V side. In the interlayer, lots of Ti(s,s) were distributed uniformly and few of Ti-Cu compounds were found, contributing to the plasticity of joints. Adding moderate Ti powder was beneficial for improving the interfacial reaction between C_f/SiC composite and filler material, which affected the lap-shear strength of joints.     

Solid-State Diffusion Bonding of Carbon–Carbon Composites with Borides and Carbides

Solid-state diffusion bonding of carbon–carbon (C─C) composites by using boride and carbide interlayers has been investigated. The interlayer materials used in this study were single-phase borides (TiB₂ or ZrB₂), eutectic mixtures of borides and carbides (ZrB₂+ ZrC or TiB₂+ B₄C), and mixtures of TiB₂+ SiC + B₄C produced in situ by chemical reactions between B₄C, Ti, and Si or between TiC, Si, and B. The double-notch shear strengths of the joints produced by solid-state reaction sintering of B₄C + Ti + Si interlayers were much higher than those of joints produced with other interlayers. The maximum strength was achieved for C─C specimens bonded at 2000°C with a 2:1:1 mole ratio of Ti, Si, and B₄C powders. The reaction products identified in the interlayers, after joining, were TiB₂, SiC, and TiC. The joint shear strength increased with the test temperature, from 8.99 MPa at room temperature to an average value of 14.51 MPa at 2000°C.     

Interfacial reactions and joining characteristics of a Cu–Pd–V system filler alloy with Cf/SiC composite

A novel composition of Cu–Pd–V filler alloy was designed for the joining of C_f/SiC composite. The filler alloy was fabricated into brazing foils with a thickness of 0.15 mm by a rolling process. The alloy′s wettability on the C_f/SiC composite was studied with the sessile drop method. After heating at 1473 K for 10 min the Cu–Pd–V filler alloy showed a low contact angle of 6° on the composite. A VC_0.75 reaction band was formed at the surface of the C_f/SiC composite under the brazing condition of 1443 K /10 min, and the microstructure in the central part of the joint was composed of (Cu, Pd) solid solution and eutectic-like phase of Pd₂Si+Cu₃Pd. The interfacial reaction mechanism is discussed. The room-temperature three-point bend strength of C_f/SiC–C_f/SiC joints brazed with Cu–Pd–V filler alloy at 1443 K for 10 min is 128 MPa, and the joint strengths at temperatures of 873–1073 K are even higher than the room-temperature strength. The presence of refractory Pd₂Si compounds within the joints should contribute to the stable high-temperature joint strengths.     

Molten salt synthesis of a SiC coating on graphite flakes for application in refractory castables

A silicon carbide coating was formed on the surface of graphite flakes by reaction of molten Si with carbon at 1100–1300 °C in a 95%KCl-5%NaF molten salt under Ar atmosphere. The effect of temperature and Si/graphite ratio in the initial mixture on the quality and the amount of SiC were investigated by XRD and SEM/EDS analyses. Also, the water wettability, oxidation resistance and zeta potential of un-coated and coated graphite were examined by TGA analysis and sedimentation test. The results show the amount of coating to increase in the coated flakes with increasing temperature and Si/graphite ratio. The SiC coating improves water wettability of graphite and acts as a protective layer to enhance oxidation resistance. The zeta potential of coated graphite was also increased which indicated a better dispersion in water based systems. These improvements in both the water dispersivity and oxidation resistance of SiC coated graphite would make it as promising candidate raw materials for application in C-containing refractory castables.     

Microstructure and joining strength evaluation of SiC/SiC joints brazed with SiCp/Ag–Cu–Ti hybrid tapes

SiC particulates were mixed with Ag–Cu–Ti powders to fabricate SiC_P/Ag–Cu–Ti (SICACT) sheets by tape casting process, which were used to braze the sintered SiC ceramics with the structure of SiC/Ag–Cu–Ti foil/SICACT sheet/Ag–Cu–Ti foil/SiC. Microstructure and joining strength both at room temperature and at high temperature were characterized by electron probe X-ray microanalyzer, electron dispersive spectroscopy, transmission electron microscopy, and flexural strength test. The SiC particulates from the SICACT sheets were randomly distributed in the filler alloy matrix and reacted with Ti from the filler alloy. Reaction products TiC and Ti₅Si₃ were found in the interfacial reaction layer. With the increase in SiC particulates volume fraction, the joining strength at room temperature first increased, and then decreased, which was affected by both CTE mismatch and the thickness of the reaction layer. In addition, the joining strength of joints brazed using SICACT sheets at 600?°C can reach 197 MPa, which was obviously higher than that brazed using Ag–Cu–Ti filler alloy.     

Production of Silicon Carbide Pieces by Immersion of Silicon Preforms in Carbonaceous Powders

In this work a novel method for production of silicon carbide (SiC) pieces, which involves the heating of silicon (Si) preforms immersed in graphite powder is presented. Such preforms were obtained via low-pressure injection molding (LPIM), although any other conformation route can be used. The process can be carried out at modest temperatures and gradients in standard furnaces used for processing other ceramics. These features make this process a simpler and cheaper alternative, when compared with other methods of SiC fabrication. The variables affecting the process have been identified, and an optimum-heating ramp has been established. Under these conditions, the obtained SiC products show no remnant-free Si, and their mechanical behavior allows their use in several less-demanding SiC applications, for which expensive high-performance SiC products are unaffordable. In the proposed chain of reactions, CO( g ) is responsible for the carburization of the pieces. All phases present are identified, and their distribution is explained by means of competitive reactions. In our opinion, this novel method can be extended to an industrial scale because it is simple and involves cheap raw materials.     

Joining of Cf/SiC composite with a Cu–Au–Pd–V brazing filler and interfacial reactions

A new Cu–Au–Pd–V filler alloy was designed for the joining of C_f/SiC composite. Its wettability on the composite was studied with the sessile drop method. After heating at 1473 K for 10 min the filler alloy showed a low contact angle of 5°. The interfacial reactions under the brazing condition of 1443 K/10 min resulted in the formation of VC_0.75 reaction band at the surface of the composite, and the microstructure in the central part of the joint is composed of Cu(Au, Pd) solid solution and Pd₂Si compound. The average three-point bend strength of the C_f/SiC–C_f/SiC joints at room temperature is 135 MPa. The joints also exhibit stable strengths at high temperatures of 873–1073 K. The presence of refractory Pd₂Si compound within the Cu(Au, Pd) solid solution matrix throughout the joint should contribute to the stable high-temperature property.     

A novel high entropy CoFeCrNiCu alloy filler to braze SiC ceramics

In order to reduce intermetallic compound formations in brazed joints, a CoFeCrNiCu high entropy alloy was invented and employed to braze SiC ceramics. Results show that SiC ceramics were tightly and strongly brazed with the CoFeCrNiCu filler. Microstructure, phase and shear strength were systematically studied for joints brazed at different temperature. Main compositions were identified as high-entropy FCC, Cu(s, s), Si(s, s), and Cr₂₃C₆ phases, regardless the brazing temperature differences. After being brazed at 1453 K, the joint reached a maximum shear strength of 60 MPa, much higher than those brazed with conventional AgCuTi filler. Thanks to high entropy effect of CoFeCrNiCu filler, random solid solution turned out in the seam and benefitted joint quality. The successful use of CoFeCrNiCu high entropy alloy as fillers can expand the application range of high entropy alloys and provide a new filler system to braze ceramics.     

Joining of SiC using CoFeCrNiCuTi high entropy alloy filler by electric current field assisted sintering

SiC ceramics were brazed by electric field-assisted sintering technology using CoFeCrNiCuTi high-entropy alloy as joining filler. The effect on the interface microstructure and bend strength of brazed joints at different brazing temperature was systemically studied. The interfacial reaction was controlled by adjusting the brazing temperature. The main components in the brazing seam are high-entropy alloys FCC (HEAF), C, TiC, CrC, and Cr₂₃C₆ phase. Furthermore, the maximum bending strength of 54 MPa was found when brazed at a lower temperature of 1125℃. In addition, due to the electric field-assisted sintering technology and the high-entropy effect of the CoFeCrNiCuTi filler, the diffusion of elements and the formation of solid solution were accelerated. This suggests that the current field was beneficial to improve the inter-diffusion between the CoFeCrNiCuTi filler and SiC ceramics. Consequently, the low-temperature rapid brazing of SiC ceramics was realized, and this technology provides a new filler system for ceramic brazing.     

Strength and Microstructure of Silicon Nitride Ceramics Brazed with Nickel-Chromium-Silicon Alloys

Joining of sintered Si₃N₄ was performed using a high-temperature brazing technique. Ni-based brazing alloys having the same Ni:Cr ratio as AWS BNi-5 (Ni·18Cr·19Si (at. %)) but different Si content were used as the brazing filler metals. Joining experiments were performed at 1220°C under a N₂ partial pressure of 15 Pa for different times between 5 to 15 min. The highest room-temperature four-point bend strength of the joints was 115 MPa, whereas 220 MPa was achieved when the joints were tested at 900°C. The high strength of the experimental joints was attributed to the reduction in residual stresses and formation of a CrN reaction layer at the ceramic/filler metal interface.     

Effect of brazing parameters on microstructure and mechanical properties of Cf/SiC and Nb-1Zr joints brazed with Ti-Co-Nb filler alloy

Reliable brazing of carbon fiber reinforced SiC (C_f/SiC) composite to Nb-1Zr alloy was achieved by adopting a novel Ti45Co45Nb10 (at.%) filler alloy. The effects of brazing temperature (1270–1320 °C) and holding time (5–30 min) on the microstructure and mechanical properties of the joints were investigated. The results show that a continuous reaction layer (Ti,Nb)C was formed at the C_f/SiC/braze interface. A TiCo and Nb(s,s) eutectic structure was observed in the brazing seam, in which some CoNb₄Si phases were distributed. By increasing the brazing temperature or extending the holding time, the reaction layer became thicker and the amount of the CoNb₄Si increased. The optimized average shear strength of 242 MPa was obtained when the joints were brazed at 1280 °C for 10 min. The high temperature shear strength of the joints reached 202 MPa and 135 MPa at 800 °C and 1000 °C, respectively.     

Processing and characterization of particles reinforced SiOC composites via pyrolysis of polysiloxane with SiC or/and Al fillers

Polysiloxane loaded with SiC as inert filler, and Al as active filler, was pyrolyzed in nitrogen to fabricate SiOC composites, and the processing and properties of the filled SiOC composites were investigated. Adding SiC fillers could reduce the linear shrinkage of filler-free cured polysiloxane in order to obtain monolithic SiC/SiOC composites. The flexural strength of SiC/SiOC composites reached 201.3 MPa at a SiC filler content of 27.6 vol.%. However, SiC/SiOC composites exhibited poor oxidation resistance, thermal shock resistance and high temperature resistance. Al fillers could react with hydrocarbon generated during polysiloxane pyrolysis at 600 °C and N₂ at 800 °C to form Al₄C₃ and AlN, respectively. The volume expansions resulting from these two reactions were in favor of the reduction in linear shrinkage and the improvement in flexural strength of SiC/SiOC composites. The flexural strength of Al-containing SiC/SiOC composites was 1.36 times that of SiC/SiOC composites without Al at an Al filler content of 20 vol.%. The addition of Al fillers remarkably improved the high temperature resistance and oxidation resistance of SiC/SiOC composites, but not thermal shock resistance.     

Interfacial microstructure and mechanical properties of SiC joints achieved by reactive air brazing using Ag-V2O5 filler

SiC ceramics are successfully brazed via reactive air brazing using Ag-V₂O₅ fillers. The wettability of SiC ceramics by Ag-V₂O₅ fillers is investigated. Interfacial microstructure of SiC joints is analyzed by scanning electron microscopy and transmission electron microscopy with energy dispersive spectroscopy. Effect of the brazing filler composition on the microstructure and mechanical properties of SiC joints is studied in detail. The V₂O₅ from the brazing fillers is found to react intensively with SiC, and the SiO₂ reaction layer with the thickness of ?7 μm is formed on the SiC surface which ensures a good wetting of the brazing filler on SiC ceramics. The brazing seam is composed of Ag and VO₂ with small amount of remaining V₂O₅. The maximum shear strength (?58 MPa) is achieved when using the optimized brazing process (Ag-8V₂O₅, 1050 ℃/30 min, the loading pressure is ?20 kPa and the cooling rate is 2 ℃/min).     

Effect of Mo and W interlayers on microstructure and mechanical properties of Si3N4–nickel-base superalloy joints

Si₃N₄/nickel-base superalloy (Inconel-625) and Si₃N₄/Si₃N₄ joints with refractory metal (W and Mo) interlayers were vacuum brazed using a Ti-active braze Cu-ABA (92.75Cu–3Si–2Al–2.25Ti) at 1317 K for 30 min with the following interlayered arrangements: Si₃N₄/Mo/W/Inconel and Si₃N₄/Mo/W/Si₃N₄. The joints exhibited Ti segregation at the Si₃N₄/Cu-ABA interface, elemental interdiffusion across the joint interfaces, and sound metallurgical bonding. Knoop microhardness profiles revealed hardness gradients across the joints that mimicked the interlayered arrangement. The compressive shear strength of Si₃N₄/Si₃N₄ joints both with and without W and Mo layers was ∼142 MPa but the strength of Si₃N₄/Inconel joints increased from ∼9 MPa for directly bonded joints without interlayers to 53.5 MPa for joints with Mo and W interlayers.     

A Si–SiC Oxidation‐resistant Coating for Carbon/Carbon Composites by Hot‐pressing Reaction Technique

A Si–SiC coating was prepared by hot‐pressing reactive sintering (HPRS) technique for protecting carbon/carbon (C/C) composites against oxidation. The Si–SiC coating has a dense and crack‐free structure with a thickness of 70–90 μm. The Si–SiC coating by HPRS has a higher SiC content and lower Si content than the coating by pressure‐less reactive sintering (PRS). It also exhibits better oxidation‐protective ability than that prepared by PRS. With hot‐pressing, the flexural strength of the Si–SiC coated C/C composites decreases from 121 MPa to 99 MPa, and the interface bonding strength increases from 6 MPa to 10 MPa.