Microstructure and mechanical properties of in situ TiB reinforced titanium matrix composites based on Ti–FeMo–B prepared by spark plasma sintering

The in situ synthesized TiB reinforced titanium matrix composites have been prepared by spark plasma sintering at 800–1200 °C under 20 MPa for 5 min. The effects of sintering temperature and reinforcement volume fraction on flexural strength, Young’s modulus and fracture toughness of the composites are investigated. The titanium matrix consists of -Ti and β-Ti phases, and the volume fraction of β-Ti increases with increasing sintering temperatures. The in situ synthesized TiB reinforcements are distributed randomly and uniformly in matrix. The transverse section of TiB has a hexagonal shape aligned along [0 1 0] direction, and the crystallographic planes of the TiB needles are always of the type . The 10 vol% TiB reinforced composite sintered at 1000 °C exhibits excellent mechanical properties. The flexural strength, Young’s modulus and fracture toughness of this composite are 1560 MPa, 137 GPa and 8.64 MPa · m^1/2, respectively.     

Mechanical properties of 3D KD-I SiCf/SiC composites with engineered fibre-matrix interfaces

Three-dimensional (3D) silicon carbide (SiC) matrix composites reinforced with KD-I SiC fibres were fabricated by precursor impregnation and pyrolysis (PIP) process. The fibre-matrix interfaces were tailored by pre-coating the as-received KD-I SiC fibres with PyC layers of different thicknesses or a layer of SiC. Interfacial characteristics and their effects on the composite mechanical properties were evaluated. The results indicate that the composite reinforced with as-received fibre possessed an interfacial shear strength of 72.1 MPa while the composite reinforced with SiC layer coated fibres had a much higher interfacial shear strength of 135.2 MPa. However, both composites showed inferior flexural strength and fracture toughness. With optimised PyC coating thickness, the interface coating led to much improved mechanical properties, i.e. a flexural strength of 420.6 MPa was achieved when the interlayer thickness is 0.1 μm, and a fracture toughness of 23.1 MPa m^1/2 was obtained for the interlayer thickness of 0.53 μm. In addition, the composites prepared by the PIP process exhibited superior mechanical properties over the composites prepared by the chemical vapour infiltration and vapour silicon infiltration (CVI-VSI) process.     

A Superplastic Al-Li-Cu-Mg-Zr Powder Alloy with High Hardness and Modulus

Structure/property studies were made on an experimental Al-3.18% Li-4.29% Cu-1.17% Mg-0.18% Zr powder alloy, which is of the low density/high modulus type. Alloy powder was made by the P&W/GPD rapid solidification rate (RSR) process, canned, and extruded to bar. The density was 2.458 × 10⁶ g/m³. The material was solution-treated, and aged at 149°C (300°F), 171°C (340°F), and 193°C (380°F), using hardness tests to determine the aging curves. Testpieces solution-treated at 516°C (961°F) showed an average yield strength (0.2% offset) of 43.3 ksi (299 MPa) and ultimate tensile strength of 50.0 ksi (345 MPa), with 1% elongation, which increased to 73.0 ksi (503 MPa) and 73.1 ksi (504 MPa), respectively, with only 0.2% elongation, on peak aging at 193°C (380°F), with a modulus of elasticity of 11.4 × 10⁶ psi (78.3 GPa). Hardness values reached 90–92 R_B on aging at 149–193°C (300–380°F). The as-extruded alloy showed superplastic behavior at 400–500°C (752–932°F) with elongations of 80–185% on 25.6 mm, peaking at 450°C (842°F). An RSR Al-2.53% Li-2.82% Mn-0.02% Zr extruded alloy showed only 18–23% elongation at 400–500°C (752–932°F).     

Strength and toughness of beryllium-niobium intermetallic compounds

Bend and compression strengths, fracture toughness, and high-temperature microhardness of Be---Nb intermetallic compounds were measured at temperatures up to 1200 °C. Be₁₂Nb and Be₁₇Nb₂ materials exhibited brittle behavior at temperatures below 1100 °C in bending and below 800 °C in compression. Hot isostatically pressed (HIP) Be₁₂Nb had the highest low-temperature strengths (250 MPa in bending and 2750 MPa in compression) resulting from its greater fracture toughness (K_IC = 4 MPa m^1/2) compared with the other Be---Nb materials, vacuum hot pressed (BHP) Be₁₂Nb, and HIP Be₁₇Nb₂, which had . Measured strengths for the HIP Be₁₂Nb were more than twice that measured for the VHP Be₁₂Nb or for HIP Be₁₇Nb₂. The HIP Be₁₂Nb also exhibited good high-temperature mechanical properties, having a bend strength of 250 MPa at 1200 °C, compared with less than 100 MPa for the VHP Be₁₂Nb. However, intergranular embrittlement was observed at intermediate temperatures, reducing the HIP Be₁₂Nb bend strength and fracture toughness below those measured for the other materials. HIP Be₁₇Nb₂ exhibited poor low-temperature properties, but high-temperature bend strengths of 740 MPa at 1100 °C and 400 MPa at 1200 °C were measured. Strength in compression was similar for all materials above 800 °C, decreasing sharply to about 600 MPa at 1000 °C and to 200 MPa at 1200 °C. Microhardness and indentation creep tests also revealed similar high-temperature behavior among the materials. Power-law creep exponents ranging from 4.1 to 6.6 and activation energies of 220–290 kJ mol⁻¹ were measured for the beryllides, with the HIP Be₁₂Nb having the highest activation energy for creep.     

An experimental study on the in situ strength of SiC fibre in unidirectional SiC/Al composites

In order to investigate the effect of strain rate and high temperature exposure on the mechanical properties of the fibre in the unidirectional fibre reinforced metal-matrix composite, in situ SiC fibre bundles are extracted from two kinds of SiC/Al composite wires, which are heat-treated at two different temperatures (exposed in the air at 400 and 600 °C for 40 min after composition). Tensile tests for these two fibre bundles are performed at different strain rates (quasi-static test: 0.001 s⁻¹, dynamic test: 200, 700, and 1200 s⁻¹) and the stress–strain curves are obtained. The experimental results show that their mechanical properties are rate-dependent, the modulus E, strength σ_b and unstable strain _b (the strain corresponding to σ_b) all increase with increasing strain rate. Compared with the mechanical properties of the original SiC fibre, those of the two in situ fibres degrade to some extent, the degradation of the in situ fibre extracted from the composite wire exposed at 600 °C (hereafter referred to as in situ fibre 2) is more serious than that of the in situ fibre extracted from the composite wire exposed at 400 °C (hereafter referred to as in situ fibre 1). The mechanism of the degradation is investigated. A bi-modal Weibull statistical constitutive equation is established to describe the stress–strain relationship of the two in situ fibre bundles. The simulated stress–strain curves agree well with the experimental results.     

Evaluation of interfacial fracture toughness of a flip-chip package and a bimaterial system by a combined experimental and numerical method

In this paper, the interfacial fracture toughness of a flip-chip package subjected to a constant concentrated line load and a bimaterial system under thermal loading condition were evaluated using a unique six-axis submicron tester, a thermal vacuum chamber and FEM modeling coupled with a high density laser moiré interferometry. The six-axis submicron tester was used to provide a constant concentrated line load, whereas the moiré interferometry technique was used to monitor the crack length during the test. In addition, a finite element technique was simultaneously used to determine the near crack tip displacement fields of the specimens. The interfacial fracture toughness and phase angle were computed by using these near tip displacement variables through the analytical energy release rate and phase angle expressions derived by authors. The interfacial fracture toughness and the phase angle of the flip-chip package considered at the interface where the passivated silicon chip meets the underfill are 35 J/m² and −65°, respectively, while the interfacial fracture toughness and the phase angle of the tested bimaterial specimen at the interface of the molding compound/silicon with the crack length of 3.3 mm under the temperature rise thermal load from room temperature (20°C) to 138°C are 20.02 J/m² and −54.8°, respectively.     

Ablation behavior of ZrB2–SiC ultra high temperature ceramics under simulated atmospheric re-entry conditions

ZrB₂–20vol%SiC ultra high temperature ceramic (UHTC) was prepared by hot-pressing. Ablation tests of the flat-face models were conducted under ground simulated atmospheric re-entry conditions using arc-jet testing with heat fluxes of 1.7 MW/m² and 5.4 MW/m² under subsonic conditions, respectively. There was little weight or configuration change after ablation at a heat flux of 1.7 MW/m². However, ZrB₂–SiC composite underwent severe ablation and whose surface temperatures exceeded 2300 °C at a heat flux of 5.4 MW/m². Sharp-shape leading edge models were ablated under supersonic conditions with the stagnation pressure and Mach number of 1.2 atm and 2.7 M, respectively, and sharp-shaped leading edge C/SiC models were also ablated under the same condition for comparison. ZrB₂–SiC composite exhibited an excellent thermal-oxidative and configurational stability in the simulated re-entry environment compared with C/SiC material. Results indicate that ZrB₂–SiC ultra high temperature ceramics are the potential candidates for leading edges. The temperature limit for UHTC is controlled by the softening and degradation of the formed oxide scale.     

Processing, microstructure and properties of C40 Mo(Si,Al)2/Al2O3 composites

The C40 Mo(Si_0.75Al_0.25)₂/Al₂O₃ composites were prepared by spark plasma sintering (SPS) of mechanically alloyed (MA) powders. The Mo(Si_0.75Al_0.25)₂/0–20 vol.% Al₂O₃ materials, showing micron and submicron composite structure, possess a hardness of 13.9–14.6 GPa but a poor toughness of 1.78–1.80 MPa m^1/2. The addition of 30 vol.% Al₂O₃ leads to the formation of the micron C40 Mo(Si_0.75Al_0.25)₂/Al₂O₃ composite with an intergranular distribution of Al₂O₃, that results in a drop of the hardness to 10.2 GPa and an improvement of the toughness to 3.67 MPa m^1/2. The transition of the cleavage facets to the intergranular fracture with the addition of Al₂O₃ is assumed as the main toughening mechanism.     

Die Rißzähigkeit und Brucharbeit von SiC-faser-verstärkten Glasmatrix-Verbundwerkstoffen: Bestimmung durch die Chevron-Kerb-Technik

Fracture Toughness and Work of Fracture of SiC-Fibre Reinforced Glass Matrix Composites: Assessment by Means of the Chevron-Notch Technique The applicability of the chevron-notch flexural technique to determine the fracture toughness and work of fracture of fiber reinforced glass matrix composites was investigated. Borosilicate glass matrix composites containing SiC-Nicalon fiber reinforcement were considered in the as-received condition and after thermal aging. The thermal aging involved exposure of the samples to temperatures in the range 500–700 °C for up to 1000 hours in Argon. To detect the onset of unstable microcracking during the chevron-notch experiments, an acoustic emission technique was used. Except for the most severe conditions investigated (600 °C, 1000 hours and 700 °C, 100 hours), the values of the fracture toughness did not change significantly, and they were in the range 19-26 MPa m^1/2, in agreement with literature results. The possible degradation mechanisms which may be activated during high-temperature aging are discussed.     

In situ synthesis mechanism and characterization of ZrB2–ZrC–SiC ultra high-temperature ceramics

The synthesis route, microstructure and properties of ZrB₂–ZrC–SiC composites prepared from a mixture of Zr–B₄C–Si powders by in situ reactive synthesis were investigated. The reactive path and synthesized mechanism of ZrB₂–ZrC–SiC composite were studied through series of pressureless heat treatments ranging from 800 °C to 1700 °C in argon. The in situ ZrB₂–ZrC–SiC composites were fabricated under different synthesis processing. The one with 88.4% relative density performed poorly in mechanical properties due to the occurring of self-propagating high-temperature synthesis (SHS). The fully dense ZrB₂–ZrC–SiC composite was obtained under the optimized synthesis processing without SHS reactions. Its Vickers hardness, flexural strength and fracture toughness were 20.22 ± 0.56 GPa, 526 ± 9 MPa and 6.70 ± 0.20 MPa m^1/2, respectively.     

Microstructure and mechanical properties of titanium carbonitride whisker reinforced β-sialon matrix composites

The microstructure, hardness, fracture toughness and thermal shock resistance were investigated for 15 vol.% TiC_0.3N_0.7 whisker reinforced β-sialon (Si_6−zAl_zO₂N_8−z with z=0.6) composites with additions of three different volume fractions 2, 5 and 20 vol.%, of an yttrium-containing glass oxynitride phase. The composites were prepared by hot pressing at 1750°C for 90 min under a uniaxial pressure of 30 MPa in nitrogen atmosphere. The TiC_0.3N_0.7 whiskers were found to survive without deteriorating in morphology or reacting with the β-sialon matrix and/or the glass phase. The TiC_0.3N_0.7 whiskers had no obvious influence on the matrix microstructure, but their presence improved both the hardness and the fracture toughness of the composites. The highest hardness was obtained for the whisker composite with 2 vol.% glass phase (H_v=18.6 GPa). The fracture toughness and thermal shock resistance improved with increasing glass content. The whisker reinforced composite containing 20 vol.% glass showed the highest fracture toughness (K_1C=6.8 MPa m^1/2). No unstable crack extension occurred during the thermal shock test of the obtained composites in the temperature interval 90-700°C, but above 700°C severe oxidation of the whiskers precludes further evaluation of thermal shock properties by the indentation-quench method applied.     

Influence of in-plane fibre orientation on mode I interlaminar fracture toughness of stitched glass/polyester composites

The influence of in-plane fibre orientation on the mode I interlaminar fracture toughness, G_Ic of unstitched and stitched glass/polyester composites is investigated in this paper. The G_Ic of planar specimens depends on the fibre orientation, θ in the layers adjacent to the fracture plane, in addition to the property of matrix material. The mode I fracture toughness and fracture behavior of unstitched and stitched 0/0, 30/−30, 45/−45, 60/−60, 90/90 and 0/90 interfaces of unidirectional fibre mats (UD) and 30/−30, 45/−45 and 90/90 interfaces of woven roving mats (WRM) are studied. WRM layer orientation is represented by the direction of warp fibres. Stitching is done by untwisted Kevlar fibre roving of Tex 175 g/km at the stitch densities (number of stitches per unit area) of 10.24 and 20.48 stitches/inch². The specimens having same stitch density, but different stitch distributions are prepared, and the influence of stitch distribution on G_Ic is studied. Double cantilever beam (DCB) tests are carried out and the G_Ic is determined using modified beam theory. The G_Ic of both unstitched and stitched specimens increases with increase in orientation angle, θ upto 45° above which it decreases. The G_Ic values of unstitched 45/−45 delamination interface is around 2.4 times that of the unstitched 0/0 interfaces. The influence of fibre orientation on G_Ic is clearly observed in unstitched specimens, whereas in the stitched specimens, stitching plays an important role in improving the G_Ic and suppresses the influence of fibre orientation; degree of suppression increases with increasing stitch density. When the value of θ is above 45°, transverse cracks are observed in the delamination interface surrounded by UD layers; while in the delamination interface surrounded by WRM layers, transverse cracks are not initiated irrespective of the fibre orientation angle.     

Effects of oxidation on surface stresses and mechanical properties of liquid phase pressureless-sintered SiC–AlN–Y2O3 ceramics

The understanding of the oxidation mechanism of 50 wt% SiC–50 wt% AlN composites obtained by means of pressureless sintering without the protective powder bed and with Y₂O₃ as sintering-aid were significantly improved by means of Raman spectroscopy. These analyses put in evidence that “amorphous carbon” started to be formed at 1300 °C as main effect of active oxidation of SiC. At higher temperature the crystallization process began and it was completed at 1500 °C when only graphite could be recognized. On the basis of these new evidences, oxidation effects on the mechanical properties of SiC–AlN–Y₂O₃ composites were defined. First of all, heat treatment in air was able to induce a compressive surface stress due to the volume gain associated to the oxidation of the intergranular phase. As a consequence apparent fracture toughness showed a value of 6.6 MPa m^1/2 after a heat treatment at 1300 °C, while at higher temperature effects of active oxidation caused a decreasing up to 4.7 MPa m^1/2. This toughening mechanism was also used to improve the resistance to thermal shock, which was evaluated by performing quenching tests. Furthermore, passive oxidation induced the healing of superficial flaws by means of the formation of -cristobalite. This phenomenon was assumed to be responsible for the increasing of the flexural strength.     

Pyroelectric properties of BST/PLT composite thick films with addition of xPbO–(1 − x)B2O3 glass

The Ba_xSr_1−xTiO₃ (BST)/Pb_1−xLa_xTiO₃ (PLT) composite thick films (20 μm) with 12 mol% amount of xPbO–(1 − x)B₂O₃ glass additives (x = 0.2, 0.35, 0.5, 0.65 and 0.8) have been prepared by screen-printing the paste onto the alumina substrates with silver bottom electrode. X-ray diffraction (XRD), scanning electron microscope (SEM) and an impedance analyzer and an electrometer were used to analyze the phase structures, morphologies and dielectric and pyroelectric properties of the composite thick films, respectively. The wetting and infiltration of the liquid phase on the particles results in the densification of the composite thick films sintered at 750 °C. Nice porous structure formed in the composite thick films with xPbO–(1 − x)B₂O₃ glass as the PbO content (x) is 0.5 ≥ x ≥ 0.35, while dense structure formed in these thick films as the PbO content (x) is 0.8 ≥ x ≥ 0.65. The volatilization of the PbO in PLT and the interdiffusion between the PLT and the glass lead to the reduction of the c-axis of the PLT phase. The operating temperature range of our composite thick films is 0–200 °C. At room temperature (20 °C), the BST/PLT composite thick films with 0.35PbO–0.65B₂O₃ glass additives provided low heat capacity and good pyroelectric figure-of-merit because of their porous structure. The pyroelectric coefficient and figure-of-merit F_D are 364 μC/(m² K) and 14.3 μPa^−1/2, respectively. These good pyroelectric properties as well as being able to produce low-cost devices make this kind of thick films a promising candidate for high-performance pyroelectric applications.     

CVD SiC fiber-reinforced barium aluminosilicate glass—ceramic matrix composites

Unidirectional CVD SiC (SCS-6) monofilament reinforced BaOAl₂O₃2SiO₂(BAS) glass—ceramic matrix composites have been fabricated by a tape lay-up method followed by hot pressing. The glass matrix flows around fibers during hot pressing resulting in nearly fully dense (95–98%) composites. Strong and tough composites having first matrix cracking stress of 250–300 MPa and ultimate flexural strength as high as 900 MPa have been obtained. Composite fracture surfaces showed fiber pullout with no chemical reaction at the fiber/matrix interface. From fiber push out, the fiber/matrix interfacial debond strength and the sliding frictional stress were determined to be 5.9 ± 1.2 MPa and 4.8 ± 0.9 MPa, respectively. The fracture surface of an uncoated SiC (SCS-0)/BAS composite also showed fiber/matrix debonding, fiber pullout, and crack deflection around the fibers implying that the SiC fibers may need no surface coating for reinforcement of the BAS glass-ceramic. Applicability of micromechanical models in predicting the first matrix cracking stress and the ultimate strength of these composites has also been examined.     

Effect of annealing on the structural and optical properties of non-coated and silica-coated ZnS:Mn nanoparticles

The Mn²⁺-doped ZnS nanoparticles stabilized by sodium citrate were synthesized through a simple chemical route. Using the ZnS:Mn nanoparticles as seeds, the silica-coated ZnS:Mn nanocomposites were formed in isopropanol by the controlled hydrolysis of tetraethyl orthosilicate. The photoluminescence spectra confirmed that the Mn²⁺ ions were incorporated into the ZnS nanoparticles. The annealing effect on the structural and optical properties of these particles was studied over a range of 100–400 °C. The results of X-ray diffraction and photoluminescence showed that the silica shell not only improved the thermal stability but also resisted the lattice-deformation and oxidation of the particles. The thermal analysis further confirmed that the non-coated ZnS:Mn nanoparticles were unstable beyond 200 °C.     

Improvements in mechanical properties of TiB2 ceramics tool materials by the dispersion of Al2O3 particles

TiB₂–Al₂O₃ composites with Ni–Mo as sintering aid have been fabricated by a hot-press technique at a lower temperature of 1530 °C for 1 h, and the mechanical properties and microstructure were investigated. The microstructure consists of dispersed Al₂O₃ particles in a fine-grained TiB₂ matrix. The addition of Al₂O₃ increases the fracture toughness up to 6.02 MPa m^1/2 at an amount of 40 vol.% Al₂O₃ and the flexural strength up to 913.86 MPa at an amount of 10 vol.% Al₂O₃. The improved flexural strength of the composites is a result of higher density than that of monolithic TiB₂. The increase of fracture toughness is a result of crack bridging by the metal grains on the boundaries, and crack deflection by weak grain boundaries due to the bad wetting characters between Ni–Mo and Al₂O₃.     

Reactions in Au/Nb bilayer thin films

The interdiffusion and intermetallic compound formation of Au/Nb bilayer thin films annealed at 200–400 °C have been investigated. The bilayer thin films were prepared by electron beam deposition. The Nb film was 50 nm thick and the Au film was 50–200 nm thick. The interdiffusion of annealed specimens was examined by measuring the electrical resistance and depth-composition profile and by transmission electron microscopy. Interdiffusion between the thin films was detected at temperatures above 325 °C in a vacuum of 10^-4 Pa. The intermetallic compound Au₂Nb₃ and other unknown phases form during annealing at over 400 °C. The apparent diffusion constants, determined from the penetration depth for annealing at 350 °C, are 3.5 × 10⁻¹⁵ m² s⁻¹ for Nb in Au and 8.6 × 110^7minus;15 m² s⁻¹ for Au in Nb. The Au surface of the bilayer films becomes uneven after annealing at over 400 °C due to the reaction.     

Effect of NiCrAlY platelets inclusion on the mechanical and thermal shock properties of glass matrix composites

NiCrAlY platelets modified glass matrix composites were prepared. Their microstructures were characterized, their Young's modulus, fracture strength in bending, Vickers hardness, and indentation toughness were measured, and their thermal shock resistance was studied using quenching-strength and indentation-quench methods. With increasing NiCrAlY content, evident enhancements of the Young's modulus and indentation toughness were obtained. The NiCrAlY alloy inclusion could exert significant influences on the retained bending strength of the samples after quench tests, from 9.6 MPa for NiCrAlY-free glass to 32.0 MPa for 30 wt.% NiCrAlY-containing composites. The indentation-quench tests showed that NiCrAlY alloy inclusion elevated the critical quenching temperatures for propagation of pre-crack, from 150 °C for NiCrAlY-free glass to 225 °C for 30 wt.% NiCrAlY-containing composites. Inclusion debonding and intersection, crack deflection and bridging were observed, and are likely the micromechanisms accounted for the improvement of fracture resistance.     

Fabrication and characterization of three-dimensional cellular-matrix composites reinforced with woven carbon fabric

A low-density three-dimensional cellular-matrix composite reinforced with woven carbon fabric (3DCMC), was fabricated by means of a pressure-quenching molding technique with nitrogen gas as the blowing agent. Epoxy resins in the interstices of yarns in the 3DCMC samples were vacated during the foaming process and needle shaped voids were also generated between fibers in yarns. The average density of the 3DCMC samples was about 10³ kg/m³, and their density reduction was 28–37% compared with a regular matrix composite with the same preform. The 3DCMC has 32–42% higher specific tensile strength, 14–37% greater specific tensile modulus, a lower specific flexure strength but 35% higher specific tangent modulus in 3-point bending, a 30–40% higher specific impact energy absorption at an impact velocity around 120 m/s and a similar specific energy absorption at about 220 m/s. Meanwhile, the 3-point bending and impact test results of 3DCMC showed that they have different fracture mechanisms from that of 3DRMC.