Toughening effect of short carbon fibers in the ZrB2–ZrSi2 ceramic composites

The toughening effect of the short carbon fibers in the ZrB₂–ZrSi₂ ceramic composites were investigated, where the ZrB₂–ZrSi₂ ceramics without carbon fibers were used as the reference. The mechanical properties were evaluated by means of flexural and SENB tests, respectively. The microstructure was characterized by SEM equipped with EDS. The results found that the short carbon fibers were uniformly incorporated in the ZrB₂–ZrSi₂ matrix and the relative density was about 97.92%. The flexural strength of short carbon fiber-reinforced ZrB₂–ZrSi₂ composites is 437 MPa; the fracture toughness and the work of fracture are 6.89 MPa m^1/2 and 259 J/m², respectively, which increased significantly in comparing with composites without fibers. The microstructure analysis revealed that the improved fracture toughness could be attributed to the fiber bridging, the fiber–matrix interface debonding and the fiber pullout, which consumed more fracture energy during the fracture process.     

Microstructure,mechanical properties,and in vitro biocompatibility of spark plasma sintered hydroxyapatite–aluminum oxide–carbon nanotube composite

In the present work, HA reinforced with Al₂O₃ and multiwalled carbon nanotubes (CNTs) is processed using spark plasma sintering (SPS). Vickers micro indentation and nanoindentation of the samples revealed contrary mechanical properties (hardness of 4.0, 6.1, and 4.4 GPa of HA, HA–Al₂O₃ and HA–Al₂O₃–CNT samples at bulk scale, while that of 8.0, 9.0, and 7.0 GPa respectively at nanoscale), owing to the difference in the interaction of the indenter with the material at two different length scales. The addition of Al₂O₃ reinforcement has been shown to enhance the indentation fracture toughness of HA matrix from 1.18 MPa m^1/2 to 2.07 MPa m^1/2. Further CNT reinforcement has increased the fracture toughness to 2.3 times (2.72 MPa m^1/2). In vitro biocompatibility of CNT reinforced HA–Al₂O₃ composite has been evaluated using MTT assay on mouse fibroblast L929 cell line. Cell adhesion and proliferation have been characterized using scanning electron microscopy (SEM), and have been quantified using UV spectrophotometer. The combination of cell viability data as well as microscopic observations of cultured surfaces suggests that SPS sintered HA–Al₂O₃–CNT composites exhibit the ability to promote cell adhesion and proliferation on their surface and prove to be promising new biocompatible materials.     

Enhanced sintering ability of biphasic calcium phosphate by polymers used for bone scaffold fabrication

Biphasic calcium phosphate (BCP), which is composed of hydroxyapatite [HAP, Ca₁₀(PO₄)₆(OH)₂] and β-tricalcium phosphate [β-TCP, β-Ca₃(PO₄)₂], is usually difficult to densify into a solid state with selective laser sintering (SLS) due to the short sintering time. In this study, the sintering ability of BCP ceramics was significantly improved by adding a small amount of polymers, by which a liquid phase was introduced during the sintering process. The effects of the polymer content, laser power and HAP/β-TCP ratios on the microstructure, chemical composition and mechanical properties of the BCP scaffolds were investigated. The results showed that the BCP scaffolds became increasingly more compact with the increase of the poly(l-lactic acid) (PLLA) content (0–1 wt.%) and laser power (6–10 W). The fracture toughness and micro-hardness of the sintered scaffolds were also improved. Moreover, PLLA could be gradually decomposed in the late sintering stages and eliminated from the final BCP scaffolds if the PLLA content was below a certain value (approximately 1 wt.% in this case). The added PLLA could not be completely eliminated when its content was further increased to 1.5 wt.% or higher because an unexpected carbon phase was detected in the sintered scaffolds. Furthermore, many pores were observed due to the removal of PLLA. Micro-cracks and micro-pores occurred when the laser power was too high (12 W). These defects resulted in a deterioration of the mechanical properties. The hardness and fracture toughness reached maximum values of 490.3 ± 10 HV and 1.72 ± 0.10 MPa m^1/2, respectively, with a PLLA content of approximately 1 wt.% and laser power of approximately 10 W. Poly(l-lactic-co-glycolic acid) (PLGA) showed similar effects on the sintering process of BCP ceramics. Rectangular, porous BCP scaffolds were fabricated based on the optimum values of the polymer content and laser power. This work may provide an experimental basis for improving the mechanical properties of BCP bone scaffolds fabricated with SLS.     

Influence of the microstructure evolution of ZrO2 fiber on the fracture toughness of ZrB2–SiC nanocomposite ceramics

ZrB₂–SiC nanocomposite ceramics toughened by ZrO₂ fiber were fabricated by spark plasma sintering (SPS) at 1700 °C. The content of ZrO₂ fiber incorporated into the ZrB₂–SiC nanocomposites ranged from 5 mass% to 20 mass%. The content, microstructure, and phase transformation of ZrO₂ fiber exhibited remarkable effects on the fracture toughness of the ZrO_2(f)/ZrB₂–SiC composites. Fracture toughness of the composites greatly improved to a maximum value of 6.56 MPa m^1/2 ± 0.3 MPa m^1/2 by the addition of 15 mass% of ZrO₂ fiber. The microstructure of the ZrO₂ fiber exhibited certain alterations after the SPS process, which enhanced crack deflection and crack bridging and affected fracture toughness. Some microcracks were induced by the phase transformation from t-ZrO₂ to m-ZrO₂, which was also an important reason behind the improvement in toughness.     

Fatigue behavior and plane-strain fracture toughness of sand-cast Mg–10Gd–3Y–0.5Zr magnesium alloy

In this study, the tensile properties, high cycle fatigue behavior and plane-strain fracture toughness of the sand-cast Mg–10Gd–3Y–0.5Zr magnesium alloy were investigated, comparison to that of sand-cast plus T6 heat treated magnesium alloy which named after sand-cast-T6. The results showed that the tensile properties of the sand-cast alloy are greatly improved after T6 heat treatment, and the fatigue strength (at 10⁷ cycles) of the sand-cast Mg–10Gd–3Y–0.5Zr magnesium alloy increases from 95 to 120 MPa after T6 heat treatment, i.e. the improvement of 26% in fatigue strength has been achieved. The plane-strain fracture toughnesses K_IC of the sand-cast and sand-cast-T6 alloys are about 12.1 and 16.3 MPa m^1/2, respectively. In addition, crack initiation, crack propagation and fracture behavior of the studied alloys after tensile test, high cycle fatigue test and plane-strain fracture toughness test were also investigated systematically.     

Mechanical properties of carbon nanotube–alumina nanocomposites synthesized by chemical vapor deposition and spark plasma sintering

Carbon nanotubes–alumina (CNT–Al₂O₃) nanocomposites with variable CNT content were directly synthesized by chemical vapor deposition (CVD). The as-grown CNT–Al₂O₃ mixture was densified by spark plasma sintering (SPS) at 1150 and 1450 °C. Vickers hardness of 9.98 GPa and fracture toughness of 4.7 MPam^1/2 were obtained for 7.39 wt.% CNT–Al₂O₃ nanocomposite. The addition of CNTs gives rise to 8.4% increase in hardness and 21.1% increase in toughness over that of the pure Al₂O₃. The optimum amount of CNTs is considered to be able to significantly enhance the mechanical property of ceramics in composites.     

Processing and electrical properties of (1 − x)[(1 − y)(Pb(Mg1/3Nb2/3)O3)–y(Pb(Yb1/2Nb1/2)O3)]–xPbTiO3 ceramics

Ferroelectric ceramics in the vicinity of morphotropic phase boundary (MPB) with compositions represented as (1 ? x)[(1 ? y)(Pb(Mg_1/3Nb_2/3)O₃)–y(Pb(Yb_1/2Nb_1/2)O₃)]–xPbTiO₃ were prepared by solid state reaction. The addition of PYbN to PMN–PT decreased the sintering temperature from 1200 °C (y = 0.25) to 1000 °C (y = 0.75). The PT content, where the MPB was observed, increased with the PYbN addition. A remanent polarization value of 28.5 µC/cm² and a coercive field value of 11 kV/cm were measured from 0.62[0.25PMN–0.75PYbN]–0.38PT ceramics, which were close to the ones measured from PMN–0.32PT ceramics. In addition, the Curie temperature was found to increase with PYbN additions.     

Structure property relation of hybrid biocomposites based on jute,viscose and polypropylene: The effect of the fibre content and the length on the fracture toughness and the fatigue properties

In the present study, the extent of jute and viscose fibre breakage during the extrusion process on the fracture toughness and the fatigue properties was investigated. The composite materials were manufactured using direct long fibre thermoplastic (D-LFT) extrusion, followed by compression moulding. The fracture toughness (K_IC) and the fracture energy (G_IC) of the PP–J30 composites were significantly improved (133% and 514%, respectively) with the addition of 10 wt% viscose fibres, indicating hindered crack propagation. The addition of viscose fibres resulted in three times higher fatigue life compared with that of the unmodified jute composites. Further, with the addition of (2 wt%) MAPP, the PP–J30–V10 resulted in a higher average viscose fibre length of 8.1 mm, and the fracture toughness and fracture energy increased from 9.1 to 10.0 MPa m^1/2 and 28.9 to 31.2 kJ/m², respectively. Similarly, the fatigue life increased 51% compared with the PP–J30–V10, thus demonstrating the increased work energy due to hindrance of the propagation of cracks.     

Development of carbon nanofiber reinforced hydroxyapatite with enhanced mechanical properties

In order to improve fracture toughness, carbon nanofibers (CNF) were used as reinforcement for hydroxyapatite (HA) composites. The powder mixture of CNF/HA were obtained with ball-milling technique. CNF/HA composites were sintered by hot-pressing with 7.81 and 15.6 MPa sintering pressure. Maximum sintering pressure was 1200 °C. Mechanical and physiological bio-compatibility were evaluated by four-point bending tests, indentation tests and immersion tests in simulated body fluid (SBF). The strength values of 10 vol.% CNF/HA composites sintered at 15.6 MPa is 90 MPa, which is within those of cortical bone. The fracture toughness values for CNF/HA composites are around 1.6 times higher than those obtained for HA. Equal bioactivity are obtained for CNF/HA composites.     

The comparison of powder characteristics and physicochemical,mechanical and biological properties between nanostructure ceramics of hydroxyapatite and fluoridated hydroxyapatite

In this study, several fluorine-substituted hydroxyapatite ceramics with the general chemical formula Ca₅(PO₄)₃(OH)_1 ? xF_x (0 ≤ x ≤ 1), where x = 0.0 (hydroxyapatite; HA), x = 0.68 (fluorhydroxyapatite; FHA) and x = 0.97 (fluorapatite; FA) were prepared. The powders were characterized using scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infra-red (FTIR), X-ray diffraction (XRD), F-selective electrode, atomic absorption spectroscopy (AAS) and EDTA titration analyses. The powders were uniaxially pressed and were formed as a disc shape. Subsequently, sinterability and thermal stability of synthesized powders were compared together. Also the effect simultaneously of fluoride content and temperature were examined on the lattice parameters and crystallites size of the obtained powders. Mechanical properties including hardness, elastic modulus and fracture toughness were measured using indentation. The in vitro dissolution studies of the samples were carried out at osteoclastic resorption conditions. Finally, the biocompatibility and cytotoxicity of the samples were carried out using osteoblast-like cells and L929 cell line, respectively. The obtained results showed that the thermal stability substantially is increased with increase incorporated fluoride into HA structure. Also it was found that the fluoride reduced the lattice parameters and crystallites size of HA. Finally, the in vitro dissolution studies results suggest that the fluoride substitutions in HA offer the ability to prepare HAs with different degrees of solubility.     

Toughening performance of glass fibre composites with core–shell rubber and silica nanoparticle modified matrices

The fracture energies of glass fibre composites with an anhydride-cured epoxy matrix modified using core–shell rubber (CSR) particles and silica nanoparticles were investigated. The quasi-isotropic laminates with a central 0°/0° ply interface were produced using resin infusion. Mode I fracture tests were performed, and scanning electron microscopy of the fracture surfaces was used to identify the toughening mechanisms.The composite toughness at initiation increased approximately linearly with increasing particle concentration, from 328 J/m² for the control to 842 J/m² with 15 wt% of CSR particles. All of the CSR particles cavitated, giving increased toughness by plastic void growth and shear yielding. However, the toughness of the silica-modified epoxies is lower as the literature shows that only 14% of the silica nanoparticles undergo debonding and void growth. The size of CSR particles had no influence on the composite toughness. The propagation toughness was dominated by the fibre toughening mechanisms, but the composites achieved full toughness transfer from the bulk.     

Superplasticity and machinability in a four-phase ceramic

Fine grained four-phase ceramic materials were fabricated to have a combination of high temperature superplasticity and room temperature machinability. The composite ceramics were made of 25 vol.% 3Y-TZP/8YSZ–25 vol.% Al₂O₃–25 vol.% MgAl₂O₄–25 vol.% LaPO₄, using LaPO₄ powders fabricated in-house. X-ray diffraction and scanning electron microscopy revealed that the grain size for the best mixed samples was in the range of 600 nm, tetragonal ZrO₂ transformed into monoclinic, and reactions in the sintered samples produced a new phase, magnetoplumbite (LaMgAl₁₁O₁₉) with lath-like grains. The formation of magnetoplumbite was facilitated by the presence of yttria and by a liquid phase generated at elevated temperatures. These four-phase ceramics had a maximum hardness of 12 GPa and fracture toughness was no more than 3 MPa√m. Deformation rates at 1400 °C under 40 MPa stress were in the superplastic range of 10^?3 s^?1 for most compositions. These four-phase ceramics were machinable as demonstrated using conventional tungsten drill bits.     

A method to measure fracture toughness of the fiber/matrix interface using the single-fiber fragmentation test

A fracture mechanics model was developed for determining the fracture toughness of the fiber/matrix (F/M) interface based on a modified test procedure for the single fiber fragmentation test (SFFT). After loading the specimen until the first fiber fracture and instantaneous debonding events occur, the specimen is unloaded and loaded again until the debond propagates. The critical load for debond propagation is measured and is used with a fracture mechanics analysis to determine the interface fracture toughness. The analysis considers also friction between the fiber and matrix in the debonded region. To obtain the necessary data for calculation of residual radial stress at the F/M interface due to matrix cure shrinkage, simultaneous measurements of dynamic modulus and cure shrinkage were conducted on the matrix (vinylester) during cure. Tests employing E-glass/vinylester SFFT specimens provided fracture toughness values of G_cd = 62 J/m² (frictionless) and 48 J/m² (friction).     

In vivo comparative property study of the bioactivity of coated Mg–3Zn–0.8Zr alloy

In this in vivo study, degradable Mg–3Zn–0.8Zr cylinders were coated with a calcium phosphorus compound (Ca–P) layer or a magnesium fluoride (MgF₂) layer; uncoated Mg–3Zn–0.8Zr alloy was used as a control. These were then implanted intramedullary into the femora of nine Japanese big-ear white rabbits for implantation periods of 1, 2 and 3 months. During the postoperative observation period with radiographic examination, the results showed that the MgF₂-coated implants were tolerated well compared to the Ca–P-coated implants and uncoated implants. Moreover, large amounts of cells, rich fibrillar collagen and calcium and phosphorus products were found on the surface of the MgF₂-coated implants using scanning electron microscopy. Micro-computed tomography further showed a slight decrease in volume (23.85%) and a greater increase in new bone mass (new bone volume fraction = 11.56%, tissue mineral density = 248.81 mg/cm³) for the MgF₂-coated implants in comparison to uncoated and Ca–P compound-coated implants after 3 months of implantation.     

Functionally graded hydroxyapatite-alumina-zirconia biocomposite: Synergy of toughness and biocompatibility

Functionally Gradient Materials (FGM) are considered as a novel concept to implement graded functionality that otherwise cannot be achieved by conventional homogeneous materials. For biomedical applications, an ideal combination of bioactivity on the material surface as well as good physical property (strength/toughness/hardness) of the bulk is required in a designed FGM structure. In this perspective, the present work aims at providing a smooth gradation of functionality (enhanced toughening of the bulk, and retained biocompatibility of the surface) in a spark plasma processed hydroxyapatite-alumina-zirconia (HAp-Al₂O₃-YSZ) FGM bio-composite. In the current work HAp (fracture toughness ~ 1.5 MPa.m^1/2) and YSZ (fracture toughness ~ 6.2 MPa.m^1/2) are coupled with a transition layer of Al₂O₃ allowing minimum gradient of mechanical properties (especially the fracture toughness ~ 3.5 MPa.m^1/2). The in vitro cyto-compatibilty of HAp-Al₂O₃-YSZ FGM was evaluated using L929 fibroblast cells and Saos-2 Osteoblast cells for their adhesion and growth. From analysis of the cell viability data, it is evident that FGM supports good cell proliferation after 2, 3, 4 days culture. The measured variation in hardness, fracture toughness and cellular adhesion across the cross section confirmed the smooth transition achieved for the FGM (HAp-Al₂O₃-YSZ) nanocomposite, i.e. enhanced bulk toughness combined with unrestricted surface bioactivity. Therefore, such designed biomaterials can serve as potential bone implants.     

Microstructure and mechanical properties of carbon fiber reinforced multilayered (PyC–SiC)n matrix composites

Carbon fiber reinforced multilayered (PyC–SiC)_n matrix (C/(PyC–SiC)_n) composites were prepared by isothermal chemical vapor infiltration. The phase compositions, microstructures and mechanical properties of the composites were investigated. The results show that the multilayered matrix consists of alternate layers of PyC and β-SiC deposited on carbon fibers. The flexural strength and toughness of C/(PyC–SiC)_n composites with a density of 1.43 g/cm³ are 204.4 MPa and 3028 kJ/m³ respectively, which are 63.4% and 133.3% higher than those of carbon/carbon composites with a density of 1.75 g/cm³. The enhanced mechanical properties of C/(PyC–SiC)_n composites are attributed to the presence of multilayered (PyC–SiC)_n matrix. Cracks deflect and propagate at both fiber/matrix and PyC–SiC interfaces resulting in a step-like fracture mode, which is conducive to fracture energy dissipation. These results demonstrate that the C/(PyC–SiC)_n composite is a promising structural material with low density and high flexural strength and toughness.     

Lead-free electrostrictive bismuth perovskite ceramics with thermally stable field-induced strains

Electric field-induced strain (EFIS) properties of Bi_1/2(Na_0.82K_0.18)_1/2TiO₃ (BNKT) ceramics modified with Sr(K_1/4Nb_3/4)O₃ (SKN) have been investigated as functions of composition and temperature. BNKT ceramics near a phase boundary revealed the coexistence of ferroelectric rhombohedral and tetragonal phases, resulting in a typical ferroelectric butterfly-shaped bipolar S–E loop at room temperature, whose normalized strain (S_max/E_max) showed a significant temperature coefficient of 0.38 pm/V/K. However, 5 mol% SKN-modified BNKT ceramics revealed a typical electrostrictive behaviour with a thermally stable electrostrictive coefficient, Q₃₃ = 0.021 m⁴/C², which is almost comparable to that of Pb(Mg_1/3Nb_2/3)O₃ (PMN) ceramics that have been dominantly used as Pb-based electrostrictive materials over the last decades.     

Piezoelectric and dielectric properties of 0.98(Na0.5K0.5)NbO3–0.02Ba(ZrxTi(1−x))O3 ceramics

Lead-free 0.98(Na_0.5K_0.5)NbO₃–0.02Ba(Zr_xTi_(1?x))O₃ (0.98NKN–0.02BZT) ceramics with Zr contents were fabricated by a conventional mixed-oxide method. The results indicate that the Zr/Ti ratio significantly influences the structural, piezoelectric, dielectric, and ferroelectric properties of 0.98NKN–0.02BZT ceramics. For the 0.98NKN–0.02BZT (x = 0) ceramics sintered at 1090 °C, the bulk density increased as the Zr contents decreased and showed a maximum value at x = 0. The Curie temperature of the 0.98NKN–0.02BZT ceramics slightly decreased as the Zr contents increased. The dielectric constant, piezoelectric constant, and electromechanical coupling factor of samples were maximized at x = 0, which might be due to the increase in density. A high d₃₃ = 194 pC/N, k_p = 38% were obtained for the 0.98NKN–0.02BZT ceramics sintered at 1090 °C for 4 h.     

Electrocaloric properties of (1 − x)Pb(Mg1/3Nb2/3)O3–xPbTiO3 ferroelectric ceramics near room temperature

Electrocaloric effects of (1 − x)Pb(Mg_1/3Nb_2/3)O₃–xPbTiO₃ [abbreviated as (1 − x)PMN–xPT] ferroelectric ceramics with x being, 0.08, 0.10, and 0.25, respectively, were measured near room temperature, and the origins of the electrocaloric effects of these ceramics were discussed. It was found that these ceramics possess large electrocaloric effect with ΔT being, more than 1 K under an electric field of 1.5 kV mm⁻¹ in a wide temperature range (more than 10 K) near room temperature, and this effect is due to both of the electrocaloric effect resulting from the electric field induced first-order phase transition and the linear electrocaloric effect. It is expected that these ceramics could be used for multi-stage cascade ferroelectric refrigeration near room temperature.     

Microstructures and fracture toughness of directionally solidified Mo–ZrC eutectic composites

Microstructures and fracture toughness of arc-melted and directionally solidified Mo–ZrC eutectic composites were investigated in this study. Two kinds of directionally solidified composites were prepared by spot-melting and floating zone-melting. Microstructure of the arc-melted composite (AMC) consists of equiaxed eutectic colonies, in which ZrC particles are dispersed. The spot-melted composite (SMC) exhibits spheroidal colony structure, which is rather inhomogeneous in size and morphology. ZrC fibers in the eutectic colonies are aligned almost parallel to the growth direction. Well aligned, homogeneous columnar structure with thin ZrC fibers evolves in the floating zone-melted composite (FZC). Texture measurement by X-ray diffractometry revealed that the growth direction of Mo solid solution (Mo_SS) in FZC is preferentially 〈100〉, while that of SMC is scattered. Fracture toughness K_Q evaluated by three point bending test using the single edge notched beam method is >13 MPa m^1/2 for AMC, 20 MPa m^1/2 for SMC and 9 MPa m^1/2 for FZC. Intergranular fracture along colony boundaries is often observed in AMC. In contrast, transgranular fracture is dominant in SMC and FZC, although significant gaps caused by intergranular fracture are occasionally observed in SEM micrographs of SMC. Fracture surface in FZC is wholly flat. Pull-out of ZrC occurs owing to Mo/ZrC interfacial debonding in intergranularly fractured regions of AMC and SMC.Coarse elongated colonies in SMC and FZC induce transgranular fracture instead of intergranular fracture. Intergranular fracture and interfacial debonding in AMC and SMC causes frequent crack deflection accompanied by ligament formation and crack branching, which is responsible for the high fracture toughness of the composites. Preferred 〈100〉 growth of Mo_SS phase in FZC leads to brittle {100} cleavage fracture associated with low fracture toughness.