Microstructure and mechanical properties of BN-Si3N4 and AlON joints brazed with Ag-Cu-Ti filler alloy

AlON was successfully brazed to BN-Si₃N₄ using a Ag-Cu-Ti filler alloy. SEM, TEM and XRD studies revealed that a TiN + TiB₂ + Ti₅Si₃ reaction layer formed adjacent to the BN-Si₃N₄ while a (Cu,Al)₃Ti₃O layer formed adjacent to the AlON. In addition, Ag-Cu eutectic, Cu(s,s) and AlCu₂Ti were observed in the brazing filler. The effect of brazing temperature on the microstructure and mechanical properties of the joints was investigated. As the brazing temperature increased, the reaction layers became thicker, while the thickness of the brazing seam decreased. Meanwhile, the amount and the size of AlCu₂Ti intermetallic compounds decreased. The shear strength of the joints first increased and then dropped with increasing the brazing temperature. A joint with a maximum strength of 94 MPa was obtained when it was brazed at 850 °C for 15 min.     

Joining and mechanical testing of oxide/oxide (Nextel ™610/alumina-zirconia) ceramic composites

Efficient joining materials and techniques are of critical importance for the integration of CMCs in high performance structures. Continuous oxide fiber Nextel^? 610/alumina-zirconia composites were successfully joined to themselves by using a novel glass-ceramic based on the SiO₂-CaO-Al₂O₃-MgO-Y₂O₃-ZrO₂ system.Crystallization kinetic of the novel glass-ceramic was studied using Matusita, Sakka and Ozawa equations. Single lap off-set shear tests and four-point bending tests were performed at room temperature and at 850 °C to investigate the mechanical strength of the joints. Thermal ageing was performed at 850 °C for 100 h in air to check the thermal stability of the joined components. The results showed that the joints were oxidation resistant and the joined interfaces were well bonded. Single lap off-set shear tests on joined samples resulted in delamination of the composites. The average flexural strengths of the joined samples were 71 MPa and 81 MPa, at room temperature and at 850 °C, respectively.     

Brazing SiC ceramic using novel B4C reinforced Ag–Cu–Ti composite filler

The development of new composite fillers is crucial for joining ceramics or ceramics to metals because the composite fillers exhibit more advantages than traditional brazing filler metal. In this research, novel B₄C reinforced Ag–Cu–Ti composite filler was developed to braze SiC ceramics. The interfacial microstructure of the joints was characterized by scanning electron microscope (SEM), X-ray diffraction (XRD) and transmission electron microscopy (TEM). The effect of B₄C addition and brazing temperature on the microstructure evolution and mechanical properties of the joints was analyzed. The results revealed that TiB whisker and TiC particles were simultaneously synthesized in the Ag-based solid solution and Cu-based solid solution due to the addition of B₄C particles. As the brazing temperature increased, the thickness of Ti₃SiC₂+Ti₅Si₃ layers adjacent to SiC ceramic increased. Desirable microstructure similar to the metal matrix reinforced by TiB whisker and TiC particles could be obtained at brazing temperature of 950 °C. The maximum bending strength of 140 MPa was reached when the joints brazed at 950 °C for 10 min, which was 48 MPa (~52%) higher than that of the joints brazed using Ag–Cu–Ti filler.     

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.     

Reaction joining of SiC ceramics using TiB2-based composites

SiC ceramics were reaction joined in the temperature range of 1450–1800 °C using TiB₂-based composites starting from four types of joining materials, namely Ti–BN, Ti–B₄C, Ti–BN–Al and Ti–B₄C–Si. XRD analysis and microstructure examination were carried out on SiC joints. It is found that the former two joining materials do not yield good bond for SiC ceramics at temperatures up to 1600 °C. However, Ti–BN–Al system results in the connection of SiC substrates at 1450 °C by the formation of TiB₂–AlN composite. Furthermore, nearly dense SiC joints with crack-free interface have been produced from Ti–BN–Al and Ti–B₄C–Si systems at 1800 °C, i.e. joints TBNA80 and TBCS80, whose average bending strengths are measured to be 65 MPa and 142 MPa, respectively. The joining mechanisms involved are also discussed.     

On the mechanical,thermophysical and dielectric properties of Nextel™ 440 fiber reinforced nitride matrix (N440/Nitride) composites

The Nextel? 440 fiber reinforced nitride matrix (N440/Nitride) composites were fabricated by precursor infiltration and pyrolysis (PIP) route. The results demonstrated that the original N440 fiber had a phase composition of amorphous SiO₂ and γ-Al₂O₃. Its single filament tensile strength was 3.03 GPa (at room temperature), while it dropped to 72.6% and 35.1% at 1200 °C and 1400 °C, respectively. The phase content of N440/Ntride composites was mainly γ-Al₂O₃ and amorphous BN, as well as mullite phase (formed at > 1100 °C). The composites owned a flexural strength up to 76.0 MPa at room temperature. The stair-stepping decrease in the load-displacement curve and fiber pull-outs in the fracture surface indicated a good fiber/matrix interface and toughness. By heating at 1400 °C, the composites still possessed 67.4% of original bending strength. It was found that the high temperatures caused strong fiber-matrix bonding and severe fiber degradation. The specific heat, CTE and thermal conductivity of the composites were 0.325–0.586 J g^?1 K^?1, (3.2–4.0) × 10^?6 K^?1 and 0.78–3.47 W m^?1 K^?1, respectively. The composites possessed a dielectric constant of 4.25–4.35 and loss tangent of 0.004–0.01 at 8–12 GHz. The good overall performances enabled the N440/Nitride composites advanced high-temperature wave-transparent applications.     

High temperature properties of the monolithic CVD β-SiC materials joined with a pre-sintered MAX phase Ti3SiC2 interlayer via solid-state diffusion bonding

Monolithic high purity CVD β-SiC materials were successfully joined with a pre-sintered Ti₃SiC₂ foil via solid-state diffusion bonding. The initial bending strength of the joints (∼ 220 MPa) did not deteriorate at 1000 °C in vacuum, and the joints retained ∼ 68 % of their initial strength at 1200 °C. Damage accumulation in the interlayer and some plastic deformation of the large Ti₃SiC₂ grains were found after testing. The activation energy of the creep deformation in the temperature range of 1000 – 1200 °C in vacuum was ∼ 521 kJmol⁻¹. During the creep, the linkage of a significant number of microcracks to form a major crack was observed in the interlayer. The Ti₃SiC₂ interlayer did not decompose up to 1300 °C in vacuum. A mild and well-localized decomposition of Ti₃SiC₂ to TiC_x was found on the top surface of the interlayer after the bending test at 1400 °C in vacuum, while the inner part remained intact.     

Microstructure and mechanical properties of ZTA composites fabricated by oscillatory pressure sintering

The influence of sintering temperature on the microstructure and mechanical properties of Al₂O₃?20 wt% ZrO₂ composites fabricated by oscillatory pressure sintering (OPS) was investigated by means of X-ray diffraction, scanning electron microscopy, three-point bending test and Vickers indentation. Results were compared to specimens obtained by conventional hot pressing (HP) under a similar sintering schedule. The optimum oscillatory pressure sintering temperature was found to be 1600 °C; almost fully dense materials (99.94% of theoretical density) with homogeneous microstructure could be achieved. The highest flexural strength, fracture toughness and hardness of such composites reached 1145 MPa, 5.74 MPa m^1/2 and 19.08 GPa when sintered at 1600 °C, respectively. Furthermore, the oscillatory pressure sintering temperature could be decreased by more than 50 °C as compared with the HP method, OPS favouring enhanced grain boundary sliding, plastic deformation and diffusion in the sintering process.     

Joining of dense Si3N4 ceramics with tape cast Lu-Al-Si-O-N interlayer

Lu-Al-Si-O-N tapes with different thickness were used to join gas pressure sintered Si₃N₄ ceramics. The microstructure of the joints and the influences of the joint thickness and joining temperature on the bonding strength of the as-joined Si₃N₄ ceramics have been investigated. The highest bonding strength about ~ 300 MPa of the joined specimens was achieved by using 450 µm interlayer at 1450 °C. The existence of Si₃N₄ nanowires was beneficial for the improvement of the bonding strength by interweaving the oxynitride glass matrix in the joint region.     

Microstructure evolution and mechanical property of ZrC-SiC/Ti6Al4V joints brazed using Ti-15Cu-15Ni filler

ZrC-SiC ceramic and TC4 alloy were successfully brazed using a self-prepared Ti-15Cu-15Ni filler. The microstructure and mechanical property of the joints obtained at different brazing temperatures were investigated. The results indicated that Ti from the Ti-15Cu-15Ni and the TC4 reacted with the ZrC-SiC to form TiC phase adjacent to the ZrC-SiC ceramic. In the brazing seam, Ti₂(Ni, Cu) intermetallic compounds zone (IMCs Zone), Hypoeutectic Zone and Hypereutectoid Zone formed. The brazing temperature affected the dissolution of TC4 into the braze filler significantly, and then determined the microstructure of the joint. The formation of α-Ti in the brazing seam could decrease the hardness and the brittleness of the brazing seam, which was beneficial to the property of the brazed joint. The joint strength reached a maximum value of 43 MPa when the joint was brazed at 970 °C and cracks propagated in the ZrC-SiC substrate near the brazing seam.     

Effect of SNNWS content on the microstructure and properties of SNNWS/Si-C-N ceramic composites via PIP

Si-C-N ceramic composites containing well distributed silicon nitride nanowires (SNNWs) were fabricated by die-pressing and precursor infiltration and pyrolysis process at a low temperature. The structure, composition, mechanical and thermophysical properties of the composites were investigated. The results show that the composites consisted of amorphous SiCN, α-Si₃N₄ and α-cristobaslite. The composites with different contents of SNNWs possessed a density of 2.02–2.07 g cm^?3 and open porosity of 7.9–9.9%. SNNWs can effectively restrain the contraction of matrix with a decrease by 25% in linear shrinkage. The composites with 3 wt% SNNWs owned the highest flexural strength (83.7 MPa) and elastic modulus (54.0 GPa) at room temperature, which increase by 13.2% and 62.3% respectively, compared with pure SiCN ceramics. The SNNWs displayed good reinforcement function at high temperature due to the fact that the composites with 7 wt% SNNWs had a 96.8% retention rate of bending strength at 1200 °C. The composites had relatively low coefficient of thermal expansion and thermal diffusivity which were less than 2.2 × 10^?6 K^?1 and 0.62 mm² s^?1, respectively.     

Interfacial microstructure and mechanical properties of porous-Si3N4 ceramic and TiAl alloy joints vacuum brazed with AgCu filler

Porous Si₃N₄ ceramic was firstly joined to TiAl alloy using an AgCu filler alloy. The effects of brazing temperature and holding time on the interfacial microstructure and mechanical properties of porous-Si₃N₄/AgCu/TiAl joints were studied. The typical interfacial microstructure of joints brazed at 880 °C for 15 min was TiAl/AlCu₂Ti/Ag-Cu eutectic/penetration layer (Ti₅Si₃+TiN, Si₃N₄, Ag (s, s), Cu (s, s))/porous-Si₃N₄. The penetration layer was formed firstly in the brazing process. With increasing brazing temperature and time, the thickness of the penetration layer increased. A large amount of element Ti was consumed in the penetration layer which suppressed the formation and growth of other intermetallic compounds. The penetration layer led the fracture to propagate in the porous Si₃N₄ ceramic substrate. The maximum shear strength was ~13.56 MPa.     

Investigation of brazing of Ba(Zn0.33Ta0.67)O3 ceramic with Ti6Al4V alloy

Feasibility of brazing Barium Zinc Tantalate (BZT) ceramics with Ti6Al4V alloy using active and non-active brazing alloy was investigated in the present study for high power RF window application. BZT ceramics were brazed successfully with Ti6Al4V alloy under high vacuum with active brazing alloy (Ticusil® (4.5%Ti) and Cusil-ABA® (1.5%Ti) at 850 °C and non-active brazing alloy (BAg8) at 830 °C. Micrographs at the interface of non-active brazed joints are free of interfacial micro-defects, and exhibit excellent physical contact and good metallurgical bonding with high diffusivity when compared to active-brazed joints. Ceramic-filler interfacial layer thickness is high for samples containing non-active filler (~25 µm) compared to the samples containing active filler materials (~9 µm and ~5 µm). The average shear strength of BZT ceramics brazed with non-active brazing alloy BAg8 is higher (~45.5 MPa) in comparison with active brazing alloys (~33 MPa and ~31 MPa). Fracture surface reveals that the failure is on ceramics side only indicating that the strength of non-active brazed joint is more compared to ceramics.     

Interfacial microstructure and mechanical properties of zirconia ceramic and niobium joints vacuum brazed with two Ag-based active filler metals

Reliable brazing of a zirconia ceramic and pure niobium was achieved by using two Ag-based active filler metals, Ag-Cu-Ti and Ag-Cu-Ti+Mo. The effects of brazing temperature, holding time, and Mo content on the interfacial microstructure and mechanical properties of ZrO₂/Nb joints were investigated. Double reaction layers of TiO and Ti₃Cu₃O formed adjacent to the ZrO₂ ceramic, whereas TiCu₄+Ti₂Cu₃+TiCu compounds appeared in the brazing interlayer. With increasing brazing temperature and time, the thickness of the Ti₃Cu₃O layer increased with consumption of the TiO layer, and the total thickness of the reaction layers increased slightly. Meanwhile, the blocky Ti-Cu compounds in the brazing interlayer tended to accumulate and grow. This microstructural evolution and its formation mechanism are discussed. The maximum shear strength was 157 MPa when the joints were brazed with Ag-Cu-Ti at 900 °C for 10 min. The microstructure and bonding properties of the brazed joints were significantly improved when Mo particles were added into the Ag-Cu-Ti. The shear strength reached 310 MPa for joints brazed with 8.0 wt% Mo additive, which was 97% higher than that of joints brazed with single Ag-Cu-Ti filler metal.     

Microtopography and mechanical properties of vacuum hot pressing Al/B4C composites

Al/B₄C composites with various volume contents of B₄C (5%, 10%, 15%, 20%, and 25%) reinforcing the Al matrix, have been fabricated by vacuum hot press sintering at 680 °C, with a soaking time of 90 min and external pressure of 30 MPa. Mechanical properties, phase composition, and microstructure of the Al/B₄C composites are discussed to reveal the physical properties of the composites. Field emission transmission electron microscopy and selected area electron diffraction have been employed to verify the interior structure and crystal growth direction, respectively. The Vickers hardness, fracture strength, tensile strength, and maximum force attained the optimal values of 108.45 ± 4.02 HV, 585.70 ± 23.26 MPa, 196.18 ± 2.48 MPa, and 4.44 ± 0.17 kN, respectively, for 25 vol% B₄C/Al composites. The static compression strength increased before the 15 vol% B₄C addition and then decreased, acquiring the highest value of 292.15 ± 2.09 MPa for 15 vol% B₄C/Al composites. In general, the relative density and ductility of these composites consistently increased, with an increase in the volume content of Al, achieving a maximum of 99.22% and 54.63 ± 7.34%, respectively, for 5 vol% B₄C/Al composites.     

Fabrication of porous Al2O3-based ceramics using ball-shaped powders by preceramic polymer process in N2 atmosphere

Porous Al₂O₃-based ceramics were successfully fabricated using ball-shaped powders by preceramic polymer process in N₂ atmosphere. These results showed that the amorphous Si-O-C ceramics were formed on the surface of ball-shaped Al₂O₃ particles by the pyrolysis of the silicone resin during sintering in N₂ atmosphere, which played a role in connecting the Al₂O₃ particles by forming the sintering necks. When the sintering temperatures increased from 1100 °C to 1600 °C, the formed Si-O-C ceramics still existed in the amorphous state and had no crystallization. Interestingly, the amorphous β-SiC formed at 1300 °C and its amount gradually increased with further increasing temperatures. The linear shrinkage rate of the samples varied from 0.49% to 0.73% and the weight loss rate increased from 2.01% to 10.77%. The apparent porosity remarkably varied with the range of 24.9% and 34.5%, as the bulk-density varied from 2.66 to 2.47 g/cm³. The bending strength gradually increased from 9.36 to 22.51 MPa with increasing temperatures from 1100 °C to 1500 °C, however, the bending strength remarkably decreased at 1600 °C, which was attributed to the comprehensive function of the high porosity, broken Al₂O₃ particles and weak connection between Al₂O₃ particles in the samples.     

Microstructure and mechanical properties of Al2O3 ceramic and TiAl alloy joints brazed with Ag–Cu–Ti filler metal

Al₂O₃ ceramic was reliably joined to TiAl alloy by active brazing using Ag–Cu–Ti filler metal, and the effects of brazing temperature, holding time, and Ti content on the microstructure and mechanical properties of Al₂O₃/TiAl joints were investigated. The typical interfacial microstructure of joints brazed at 880 °C for 10 min was Al₂O₃/Ti₃(Cu,Al)₃O/Ag(s.s)+AlCu₂Ti+Ti(Cu,Al)+Cu(s.s)/AlCu₂Ti+AlCuTi/TiAl alloy. With increasing brazing temperature and time, the thickness of the Ti₃(Cu,Al)₃O reaction layer increased, and the blocky AlCu₂Ti compounds aggregated and grew gradually. The Ti dissolved from the TiAl substrate was sufficient to react with Al₂O₃ ceramic to form a thin Ti₃(Cu,Al)₃O layer when Ag–Cu eutectic alloy was used, but the dissolution of TiAl alloy was inhibited with an increase in Ti content in the brazing filler. Ti and Al dissolved from the TiAl alloy had a strong influence on the microstructural evolution of the Al₂O₃/TiAl joints, and the mechanism is discussed. The maximum shear strength was 94 MPa when the joints were brazed with commercial Ag–Cu–Ti filler metal, while it reached 102 MPa for the joint brazed with Ag–Cu+2 wt% TiH₂ at 880 °C for 10 min. Fractures propagated primarily in the Al₂O₃ substrate and partially along the reaction layer.     

In-Situ synthesized TiC nano-flakes reinforced C/C composite-Nb brazed joint

Brazing C/C composite to Nb is often associated with the problem of high residual stress, resulting in low-strength joints. To overcome these problems, here we carried out a simple polymer carbonization process to acquire uniform carbon-covered Cu foam composite interlayer, which was subsequently used for soundly brazing C/C composite and Nb with the assembly of C/C composite/Ag-Cu-Ti foil/C-Cu foam/Ag-Cu-Ti foil/Nb. Microstructure and mechanical properties of the joints were well investigated. The carbonization reacted with Ti elements, forming uniformly distributed in-situ TiC nano-flakes in the joint seam by virtue of the porous Cu foam skeleton. Results present that the in-situ TiC nano-flakes not only greatly reduced the thermal expansion coefficient but also effectively impeded the Cu solid solutions agglomeration. The average shear strength of the joint brazed with 3% C-Cu (wt.%) foam interlayer reached ～52.8 MPa with the brazing temperature of 880 °C for 10 min.     

Dynamic oxidation and protection of the PAN pre-oxidized fiber C/C composites

Pre-oxidized fibers as reinforcement are candidates for reducing the overall cost of C/C composites with superior properties. This study investigated the dynamic oxidation and protection of the pre-oxidized fiber C/C composites (Pr-Ox-C-C). According to the Arrhenius equation, the oxidation kinetics of the Pr-Ox-C-C consisted of two different oxidation mechanism with the transition point was at about 700 °C. Scanning electron microscopy investigation showed that oxidation initiated from the fiber/matrix interface of composites, whereas the matrix carbon was easily oxidized. To improve the anti-oxidant properties of Pr-Ox-C-C, a ceramic powder-modified organic silicone resin/ZrB₂-SiC coating was prepared by the slurry method. The coated samples were subjected to isothermal oxidation for 320 h at 700 °C, 800 °C, 900 °C, 1000 °C and 1100 °C with incurred weight losses of ? 1.6%, 0.77%, ? 1.28%, 0.68% and 1.19%, respectively. After 110 cycles of thermal shock between 1100 °C and room temperature, a weight loss of 1.30% was obtained. The Arrhenius curve presented four different phases and mechanisms for coating oxidation kinetics. The excellent oxidation resistance properties of the prepared coating could be attributed to the inner layer which was able to form B₂O₃-Cr₂O₃-SiO₂ glass to cure cracks, and the ZrB₂-SiC outer layer that could provide protective oxides to reduce oxygen infiltration and to seal bubbles.     

Ultra-high elevated temperature strength of TiB2-based ceramics consolidated by spark plasma sintering

Spark plasma sintering of TiB₂–boron ceramics using commercially available raw powders is reported. The B₄C phase developed during reaction-driven consolidation at 1900 °C. The newly formed grains were located at the grain junctions and the triple point of TiB₂ grains, forming a covalent and stiff skeleton of B₄C. The flexural strength of the TiB₂–10 wt.% boron ceramic composites reached 910 MPa at room temperature and 1105 MPa at 1600 °С. Which is the highest strength reported for non-oxide ceramics at 1600 °C. This was followed by a rapid decrease at 1800 °C to 480–620 MPa, which was confirmed by increased number of cavitated titanium diboride grains observed after flexural strength tests.