Effect of PyC interphase thickness on mechanical and ablation properties of 3D Cf/ZrC–SiC composite

Three-dimensional (3D) C_f/ZrC–SiC composites were successfully prepared by the polymer infiltration and pyrolysis (PIP) process using polycarbosilane (PCS) and a novel ZrC precursor. The effects of PyC interphase of different thicknesses on the mechanical and ablation properties were evaluated. The results indicate that the C_f/ZrC–SiC composites without and with a thin PyC interlayer of 0.15 µm possess much poor flexural strength and fracture toughness. The flexural strength grows with the increase of PyC layer thickness from 0.3 to 1.2 µm. However, the strength starts to decrease with the further increase of the PyC coating thickness to 2.2 µm. The highest flexural strength of 272.3±29.0 MPa and fracture toughness of 10.4±0.7 MPa m^1/2 were achieved for the composites with a 1.2 µm thick PyC coating. Moreover, the use of thicker PyC layer deteriorates the ablation properties of the C_f/ZrC–SiC composites slightly and the ZrO₂ scale acts as an anti-ablation component during the testing.     

Microstructure and mechanical properties of ZrB2–SiC porous ceramic by camphene-based freeze casting

Camphene-based freeze casting technique was adopted to fabricate ZrB₂–SiC porous ceramic with 3-dimensional (3D) pore network. ZrB₂–SiC/camphene slurries (initial solid loading: 20 vol%, 25 vol% and 30 vol%) were prepared for freeze casting. Regardless of initial solid loading, the fabricated sample had dense/porous dual microstructure. The thickness of dense layer was about 200–300 μm. The microstructures of ZrB₂–SiC porous ceramics were significantly influenced by the initial solid loading, which determines the pore size, porosity and mechanical properties of the final products.     

Microstructure,mechanical and anti-ablation properties of SiCnw/PyC core-shell networks reinforced C/C–ZrC–SiC composites fabricated by a multistep method of chemical liquid-vapor deposition

C/C–ZrC–SiC composites reinforced by SiC nanowire (SiCnw)/pyrocarbon (PyC) core-shell networks were prepared by a multistep method of chemical liquid-vapor deposition (CLVD). The microstructure, mechanical property and ablation resistance were researched. The investigations presented that the PyC was deposited on the SiC nanowires, and the micro-scale core-shell structures were produced. Moreover, these micro-scale structures not only connected with the fibers and matrices, but also filled the pores in the composites. In contrast with C/C–ZrC–SiC composites, the flexural modulus and strength of SiCnw/PyC-C/C–ZrC–SiC composites increased by 36.91% and 44.53%, and the fracture mode was changed from the brittle to pseudo-plastic fracture. After the oxyacetylene torch ablation at two temperatures for 90s, the composites strengthened by SiCnw/PyC core-shell possessed a better resistant ablation. At ablation temperature of 2300 °C, the mass loss rate and linear reduction rate of the composites with core-shell networks decreased by 66.18% and 57.55% in contrast with the non-reinforced composites, and declined by 56.46% and 57.48% at ablation temperature of 3000 °C. The obvious decrease of ablation rates was ascribed to the dense microstructure, the small coefficient of thermal expansion (CTE), the good thermal conductivity, and the resistant ablation roles of SiCnw/PyC core-shell systems.     

Microstructure,mechanical and tribological properties of Mo–V–Cu–N coatings prepared by HIPIMS technique

A combination of high wear-resistance and low-friction is crucial for improving the wear performance of self-lubricating coatings, which is generally determined by an excellent lubricating effect and mechanical strength. In this study, the Mo–V–Cu–N coatings were prepared by HIPIMS technique with a spliced target of Mo–V–Cu at various charge voltages. The results revealed that Mo–V–Cu–N coatings presented a solid solution phase of B1–MoVN with (200) preferred orientation, and the preferred orientation was enhanced at high charge voltages. Whereas the Cu atoms formed an amorphous phase in Mo–V–Cu–N coatings due to a low Cu content of 2.3–3.6 at.%. As the charge voltage increased to 750 V, more charged metallic ions were accelerated and bombarded substrate surface efficiently, forming smooth and dense Mo–V–Cu–N coatings with a high hardness of 31.0 GPa. All the coatings presented a low friction coefficient of 0.34–0.39 due to the formation of MoO₂, VO₂ and CuO mixed oxides, and the wear mechanism was dominated by abrasive and tribo-oxidation wear at room temperature.     

Microstructure and mechanical properties of B4C–TiB2 ceramic composites prepared via a two-step method

B₄C–TiB₂ ceramic composites were fabricated by a two-step method. First, B₄C–TiB₂ composite powders were synthesized from TiC–B powder mixtures at 1400 ℃, then mixed with commercial B₄C powders by ball milling and the B₄C–TiB₂ ceramic composites were prepared by hot pressing at 1950 ℃. This two-step method not only effectively refined TiB₂ grains, but also allowed the composition of the composites to be freely designed. The microstructure and mechanical properties of the composites were investigated. The results showed that the B₄C–TiB₂ ceramic composite with a 10 wt% TiB₂ content obtained the ideal comprehensive performance, with a volume density, Vickers hardness, bending strength, and fracture toughness of 2.61 g/cm³, 35.3 GPa, 708 MPa, and 5.82 MPa m^1/2, respectively. The advantages of the in-situ reaction process were fully exerted by the two-step method, which made a remarkable contribution to the excellent properties of B₄C–TiB₂ ceramic composites.     

Microstructure,mechanical and tribological properties of Ti–B–C–N films prepared by reactive magnetron sputtering

Quaternary Ti–B–C–N thin films are deposited on high-speed steel substrates by the reactive magnetron sputtering (RMS) technique. The microstructure, mechanical and tribological properties of Ti–B–C–N films with different carbon contents (from 28.9 at.% to 54.2 at.%) are explored systematically. The microstructure of Ti–B–C–N films deposited by RMS is consisted mainly of Ti(C, N) nano-crystals embedded into an amorphous matrix of a-C/a-CN/a-BN/a-BC. As the carbon content increases, the crystalline size of the films diminishes, but the hardness linearly increases from 14 GPa to 26 GPa. The friction coefficient of the films sliding against steel GCr15 balls in air decreases with the increase of carbon content, which shows that Ti–B–C–N films with both higher hardness and lower friction coefficient can be obtained by means of increasing the carbon concentration in the films.     

Microstructure and mechanical properties of Ti–C–TiN-reinforced Ni204-based laser-cladding composite coating

In situ Ti(C, N), ring phase, and multi-phase enhanced Ni204-based alloy coating were prepared by adding various Ti/C/TiN ratios particles. The effects of the reinforcement phase on the microstructure, microhardness, tribological property, and microstructure characteristics at the interface between the coating and substrate were investigated. The results show that the coatings with a 5:1 mass fraction ratio of TiN/C exhibits the highest microhardness, which is 3.78 times higher than that of the original Ni204 coating. While, the coating with 21:7:2 mass fraction ratio of TiN/Ti/C exhibits the lowest friction coefficient, which is 4.44 times smaller than that of the original Ni204 coating. The addition of Ti and C particles promotes the precipitation of ring phase and carbides, reduces ceramic agglomeration, alleviates the floating of ceramic particles, and improves the bonding strength of reinforcement phases. Owing to the good mutual solubility among Fe, Ni, and, Cr elements, the diffusion happened at the interface between the coating and substrate.     

Microstructure and mechanical properties of Al2O3–Ti(C,N)–cBN composites prepared by a novel hot-forging process

Al₂O₃–cBN has received considerable attention in the field of ceramic cutting tools due to its high hardness, high wear resistance, and low cost, but poor interfacial bonding affects the performance of the composite. In this study, a novel hot-forging process was used to prepare high-performance Al₂O₃–cBN composites using Ti(C,N) as a binder. The evolution of the morphology, phase, and microstructure of the hot-forged Al₂O₃–Ti(C,N)–cBN composites was determined, and the mechanical properties were measured. The relative density of the composites increases significantly after hot forging, and the deformation of the composites increases with the hot-forging temperature. The highest performing Al₂O₃–Ti(C,N)–cBN composite was prepared by hot forging at 1600°C and has a hardness of 20 GPa, a bending strength of 647 MPa and a fracture toughness of 5.37 MPa m^1/2, which are superior to those of a directly hot-pressed sintered composite. However, at hot-forging temperatures higher than 1700°C, Al₅O₆N and TiB₂ are formed in the composite. In the composite hot forged at 1800°C, serrated grain boundaries promote the strength and toughness of the composite to 877 MPa and 6.76 MPa m^1/2, respectively. Therefore, the novel hot-forging process is expected to enhance material properties.     

Fiber/matrix interfacial shear strength of C/C composites with PyC–TaC–PyC and PyC–SiC–TaC–PyC multi-interlayers

The fiber/matrix (F/M) interfacial shear strength (IFSS) of carbon/carbon (C/C) composites with PyC–TaC–PyC and PyC–SiC–TaC–PyC multi-interlayers was investigated. To obtain C/C composites with PyC–TaC–PyC and PyC–SiC–TaC–PyC multi-interlayers, a thin layer of PyC was deposited on carbon fibers. After this, TaC and SiC–TaC layer(s) were uniformly deposited on the PyC coated carbon fibers. As an outer-layer, a PyC layer was deposited on these TaC and/or SiC–TaC coated carbon fibers by isothermal chemical vapour infiltration (CVI) and then densified with resin carbon by impregnation and carbonization. Finally, C/C composites with PyC–TaC–PyC and PyC–SiC–TaC–PyC multi-interlayers were obtained. The effects of PyC–TaC–PyC and PyC–SiC–TaC–PyC multi-interlayers on interfacial shear strength (IFSS) of C/C composites were investigated. Single fiber push-out tests were conducted on the fibers aligned perpendicularly on the thin slices specimen surface using nano-indentation. Results showed that the IFSS of C/C composites decreased with the introduction of PyC–TaC–PyC and PyC–SiC–TaC–PyC multi-interlayers. After heat treatment (at temperatures ranging from 1400 to 2500 °C) of C/C composites with PyC–TaC–PyC multi-interlayers, it was found that the IFSS decreased with the increase in temperature. This decrease in IFSS is explained by taking into account the microstructural variations on heat treatment.     

Microstructures and mechanical properties of functionally graded TiCN–TaC ceramics prepared by a novel layer processing strategy

Functionally graded TiCN–TaC ceramics (FGTTCs) were fabricated using a novel layer processing method based on a vacuum hot-press sintering technology. Microstructural investigations revealed a visibly layered structure for the FGTTCs with relatively flat boundaries between the neighboring layers; additionally, the layer thickness was facilely controlled. With an increase in the sintering temperature, the hardness and flexural strength of the surface and middle layers of the FGTTCs initially increased, and then decreased. The fracture toughness of the surface layer did not undergo significant changes after sintering at various temperatures, except at 1500 °C. The FGTTC sintered at 1350 °C contained uniform fine grains and simultaneously exhibited transgranular and intergranular fracture modes. Further, it presented excellent comprehensive mechanical properties, i.e., surface layer hardness = 20.28 ± 0.18 GPa, flexural strength = 1553.76 ± 22 MPa, surface layer fracture toughness = 7.29 ± 0.24 MPa m^1/2. Under the same sintering conditions, our FGTTCs presented superior mechanical properties against homogeneous TiCN–TaC ceramics (HTTCs), achieving a considerably higher flexural strength (1553.76 ± 22 vs 953.35 ± 24 MPa).     

Microstructure and mechanical properties at room and elevated temperatures of reactively hot pressed TiB2–TiC–SiC composite ceramic tool materials

TiB₂-based composite ceramic tool materials with different amounts of TiC and SiC were fabricated via a reactive hot pressing process. The mechanical properties at room temperature and flexural strength at 800–1300 °C were tested in ambient air. The composition and microstructure before and after the high-temperature strength tests were studied by X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) equipped with an energy-dispersive spectrometer (EDS). The flexural strength increment/degradation mechanisms at elevated temperatures were investigated. In-situ synthesized TiC improved the sinterability and mechanical properties of the materials at both room and elevated temperatures. Comparing with TTS (TiB₂–15.9 wt%TiC–10.6 wt%SiC) and TS (TiB₂–22.4 wt%SiC), TTS3 (TiB₂–8.1 wt%TiC–16.4 wt%SiC) had the optimum room temperature mechanical properties, i.e., flexural strength of 862 MPa, fracture toughness of 6.4 MPa m^1/2, hardness of 22.8 GPa, and relative density of 99.3%. The improved mechanical properties were ascribed to the fine grain size. The flexural strength of the TTS composite at 800 °C was higher than that at room temperature. The improvement of the flexural strength was attributed to the healing of preexisting flaws and the relief of residual stress. Substantial strength degradation took place when the temperature exceeded 1000 °C, due to softening of the grain boundaries, surface oxidation and elastic modulus degradation.     

Microstructure and mechanical properties of WC–C nanocomposite films

WC–C nanocomposite film was prepared by using a hybrid deposition system of r.f.-PACVD and DC magnetron sputtering. W concentration in the film was varied from 5.2 to 42 at.% by changing the CH₄ fraction of the mixture sputtering gas of Ar and CH₄. Hardness, residual compressive stress and electrical resistivity were characterized as a function of W concentration. Raman spectroscopy, XRD and high resolution TEM were employed to analyze the structural change in the film for various W concentrations. In the present W concentration range, the film was composed of nano-sized WC particles of diameter less than 5 nm and hydrogenated amorphous carbon matrix. Content of the WC particles increased with increasing W concentration. However, the mechanical properties of the film increased only when the W concentration was higher than 13 at.%. Structural analysis and electrical conductance measurements evidently showed that the increase in hardness and residual stress occurred as the WC particles were in contact with each other in the amorphous carbon matrix.     

Influence of graphite nano-flakes on densification and mechanical properties of hot-pressed ZrB2–SiC composite

Hot pressed monolithic ZrB₂ ceramic (Z), ZrB₂–20 vol% SiC composite (ZS₂₀) and ZrB₂–20 vol% SiC–10 vol% nano-graphite composite (ZS₂₀G_n10) were investigated to determine the influence of graphite nano-flakes on the sintering process, microstructure, and mechanical properties (Vickers hardness and fracture toughness) of ZrB₂–SiC composites. Hot pressing at 1850 °C for 60 min under 20 MPa resulted in a fully dense ZS₂₀G_n10 composite (relative density: 99.6%). The results disclosed that the grain growth of ZrB₂ matrix was efficiently hindered by SiC particles as well as graphite nano-flakes. The fracture toughness of ZS₂₀G_n10 composite (7.1 MPa m^1/2) was essentially improved by incorporating the reinforcements into the ZrB₂ matrix, which was greater than that of Z ceramic (1.8 MPa m^1/2) and ZS₂₀ composite (3.8 MPa m^1/2). The fractographical observations revealed that some graphite nano-flakes were kept in the ZS₂₀G_n10 microstructure, besides SiC grains, which led to toughening of the composite through graphite nano-flakes pull out. Other toughening mechanisms such as crack deflection and branching as well as crack bridging, due to the thermal residual stresses in the interfaces, were also observed in the polished surface.     

Microstructure and mechanical properties of α/β-Si3N4 composite ceramics with novel ternary additives prepared via spark plasma sintering

In this study, α/β-Si₃N₄ composite ceramics with high hardness and toughness were fabricated by adopting two different novel ternary additives, ZrN–AlN–Al₂O₃/Y₂O₃, and spark plasma sintering at 1550 °C under 40 MPa. The phase composition, microstructure, grain distribution, crack propagation process and mechanical properties of sintered bulk were investigated. Results demonstrated that the sintered α/β-Si₃N₄ composite ceramics with ZrN–AlN–Al₂O₃ contained the most α phase, which resulted in a maximum Vickers hardness of 18.41 ± 0.31 GPa. In the α/β-Si₃N₄ composite ceramics with ZrN–AlN–Y₂O₃ additives, Zr₃AlN MAX-phase and ZrO phase were found and their formation mechanisms were explained. The fracture appearance presented coarser elongated β-Si₃N₄ grains and denser microstructure when 20 wt% TiC particles were mixed into Si₃N₄ matrix, meanwhile, exhibited maximum mean grain diameter of 0.98 ± 0.24 μm. As a result, the compact α/β-Si₃N₄ composite ceramics containing ZrN–AlN–Y₂O₃ additives and TiC particles displayed the optimal bending strength and fracture toughness of 822.63 ± 28.75 MPa and 8.53 ± 0.21 MPa?m^1/2, respectively. Moreover, the synergistic toughening of rod-like β-Si₃N₄ grains and TiC reinforced particles revealed the beneficial effect on the enhanced fracture toughness of Si₃N₄ ceramic matrix.     

Thermophysical properties of carbon fiber reinforced multilayered (PyC–SiC)n matrix composites

Three kinds of carbon fiber reinforced multilayered (PyC–SiC)_n matrix (C/(PyC–SiC)_n) composites (n = 1, 2 and 4) were prepared by means of layer-by-layer deposition of PyC and SiC via chemical vapor infiltration. Thermal expansion behaviors in the temperature range of 800–2500 °C and thermal conductivity from room temperature to 1900 °C of C/(PyC–SiC)_n composites with various microstructures were investigated. The results show that with increasing PyC–SiC sequences number (n), the coefficients of thermal expansion of the composites decrease due to the increase of interfacial delamination, providing room for thermal expansion. The thermal diffusivity and thermal conductivity also decrease with the increase of sequences number, which are attributed to the enhancement of phonon-interface scattering resulted from the increasing number of interfaces. Modified parallel and series models considering the interfacial thermal resistance are proposed to elaborate thermal conductivity of the composites, which is in accordance with the experimental results.     

Microstructure and properties of ablative C/ZrC–SiC composites prepared by reactive melt infiltration of zirconium and vapour silicon infiltration

C/ZrC-SiC composites with a density of 3.09 g/cm³ and a porosity of 4.8% were prepared by reactive melt infiltration and vapour silicon infiltration. The flexural strength and modulus were 235 MPa and 18.3 GPa, respectively, and the fracture toughness was 7.0 MPa m^1/2. The formation of SiC and ZrSi₂ during vapour silicon infiltration, at the residual cracks and pores in the C/ZrC, enhanced the interface strength and its mechanical properties. The high flexural strength (223 MPa, c. 95% of the original value) after oxidation at 1600 °C for 10 min indicated the excellent oxidation resistance of the composites after vapour silicon infiltration. The mass loss and linear recession rate of the composites were 0.0071 g/s and 0.0047 mm/s, respectively and a fine ablation morphology was obtained.     

Microstructure and properties of CaO–ZrO2–SiO2 glass–ceramics prepared by sintering

For the development of a new wear resistant and chemically stable glass-ceramic glaze, the CaO–ZrO₂–SiO₂ system was studied. Compositions consisting of CaO, ZrO₂, and SiO₂ were used for frit, which formed a glass-ceramic under a single stage heat treatment in electric furnace. In the sintered glass-ceramic, wollastonite (CaSiO₃) and calcium zirconium silicate (Ca₂ZrSi₄O₁₂) were crystalline phases composed of surface and internal crystals in the microstructure. The internal crystal formed with nuclei having a composition of Ca_1.2Si_4.3Zr_0.2O₈. The CaO–ZrO₂–SiO₂ system showed good properties in wear and chemical resistance because the Ca₂ZrSi₄O₁₂ crystals positively affected physical and mechanical properties.     

Microstructure and mechanical properties of Al2O3–20 wt%Al2TiO5 composite prepared from alumina and titania nanopowders

In the present work, Al₂O₃–20 wt%Al₂TiO₅ composite was prepared from reaction sintering of alumina and titania nanopowders. The nano-sized raw powders were reconstituted into nanostructured particles by ball milling. Then, the nanostructured reconstituted powders were pressed and pressureless-sintered into bulk ceramics at 1300, 1400, 1500 °C for 2 h. The phase composition and microstructures of reconstituted powders and as-prepared ceramic composites were characterized by using X-ray diffractometer (XRD), scanning electron microscope (SEM), transmission electron microscope and energy-dispersive spectrometer (EDS). The microstructural analysis of the ceramic showed that the average grain size of the alumina–aluminium titanate composite increases with increasing the temperature. Also, SEM proved the existence of a proper interface between Al₂TiO₅ and Al₂O₃ grains and preferential distribution of aluminium titanate particles in the grain boundaries. XRD analysis indicated the absence of rutile titania in the sintered composite ensuring complete formation of aluminium titanate. The hardness of the samples sintered at 1300, 1400, 1500 °C were 4.8, 6.2 and 8.5 GPa, respectively.     

Microstructure,mechanical, thermal,and oxidation properties of a Zr2[Al(Si)]4C5–SiC composite prepared by in situ reaction/hot-pressing

The microstructure, mechanical and thermal properties, as well as oxidation behavior, of in situ hot-pressed Zr₂[Al(Si)]₄C₅–30 vol.% SiC composite have been characterized. The microstructure is composed of elongated Zr₂[Al(Si)]₄C₅ grains and embedded SiC particles. The composite shows superior hardness (Vickers hardness of 16.4 GPa), stiffness (Young's modulus of 386 GPa), strength (bending strength of 353 MPa), and toughness (fracture toughness of 6.62 MPa m^1/2) compared to a monolithic Zr₂[Al(Si)]₄C₅ ceramic. Stiffness is maintained up to 1600 °C (323 GPa) due to clean grain boundaries with no glassy phase. The composite also exhibits higher specific heat capacity and thermal conductivity as well as better oxidation resistance compared to Zr₂[Al(Si)]₄C₅.     

Microstructure and properties of ZrB2–SiC composites prepared by spark plasma sintering using TaSi2 as sintering additive

ZrB₂–SiC composites were fabricated by spark plasma sintering (SPS) using TaSi₂ as sintering additive. The volume content of SiC was in a range of 10–30% and that of TaSi₂ was 10–20% in the initial compositions. The composites could be densified at 1600 °C and the core–shell structure with the core being ZrB₂ and the shell containing both Ta and Zr as (Zr,Ta)B₂ appeared in the samples. When the sintering temperature was increased up to 1800 °C, only (Zr,Ta)B₂ and SiC phases could be detected in the samples and the core–shell structure disappeared. Generally, the composites with core–shell structure and fine-grained microstructure showed the higher electrical conductivity and Vickers hardness. The completely solid soluted composites with coarse-grained microstructure had the higher thermal conductivity and Young's modulus.