Densification and mechanical properties of fine-grained Al2O3-ZrO2 composites consolidated by spark plasma sintering

Alumina matrix composites containing 5 and 10 wt% of ZrO₂ were sintered under 100 MPa pressure by spark plasma sintering process. Alumina powder with an average particle size of 600 nm and yttria-stabilized zirconia with 16 at% of Y₂O₃ and with a particle size of 40 nm were used as starting materials. The influence of ZrO₂ content and sintering temperature on microstructures and mechanical properties of the composites were investigated. All samples could be fully densified at a temperature lower than 1400 °C. The microstructure analysis indicated that the alumina grains had no significant growth (alumina size controlled in submicron level 0.66-0.79 μm), indicating that the zirconia particles provided a hindering effect on the grain growth of alumina. Vickers hardness and fracture toughness of composites increased with increasing ZrO₂ content, and the samples containing 10 wt% of ZrO₂ had the highest Vickers hardness of 18 GPa (5 kg load) and fracture toughness of 5.1 MPa m^1/2.     

Compressive strength, hardness and fracture toughness of Al2O3 whiskers reinforced ZTA and ATZ nanocomposites: Weibull analysis

The aim of this investigation was to study the variability in compressive strength, fracture toughness and microhardness applying the well-known Weibull statistics and to be able to provide a wide spectrum of mechanical properties in Al₂O₃ whisker reinforced alumina toughened zirconia (ATZ) and zirconia toughened alumina (ZTA) nanocomposites for possible dental applications. Uniaxial compression tests at room temperature of samples 6.35 ± 0.03 mm in diameter and 12.50 ± 0.63 mm in length and Vickers hardness measurements on polished surfaces were carried out. The indentation fracture toughness (K_IC) was derived from the average crack length. Weibull analysis was performed on the data. The ATZ2 (18.0 wt.% Al₂O₃ + 2.0 wt.%_(w) + 80.0 wt.% ZrO₂ (TZ-3Y)) nanocomposite reported the highest average compressive load of 1200 MPa, the highest value of characteristic strength, σ_o, of 1340 MPa with Weibull modulus of 3.25 and relatively high fracture toughness (4.7 ± 0.7 MPa m^1/2), suggesting that with the wide range of mechanical properties obtained in our work, different dental applications could be offered without lead to premature failure.     

Understanding the mechanical reinforcement of uniformly dispersed multiwalled carbon nanotubes in alumino-borosilicate glass ceramic

The improvement of mechanical properties of carbon nanotube–reinforced polycrystalline ceramic or glass matrix composites was limited in earlier studies by the difficulties in producing a good dispersion of carbon nanotubes. Additionally, a proper understanding of the reinforcing mechanisms, if any, affecting the mechanical properties of ceramics containing carbon nanotubes is still lacking. We report here the effects of a good dispersion of as much as 10 wt.% multiwalled carbon nanotubes (MWCNTs) on the mechanical properties of dense alumino-borosilicate glass ceramics (ABS) prepared by an ultrasonication-assisted sol–gel technique followed by hot pressing (950 °C; 2 h; Ar atmosphere). The fracture toughness and flexural strength of the nanocomposites increased with increasing MWCNT content up to 10 wt.%. The ABS–10 wt.% MWCNT nanocomposite possessed nearly double the strength of the unreinforced ABS, accompanied by ～150% improvement in fracture toughness. However, a further increase in MWCNT content to 15 wt.% resulted in a modest deterioration of the mechanical properties due to agglomeration of the MWCNTs. The carbon nanotubes have been observed to bridge crack openings of the order of ～100 nm and the experimental evidence, along with theoretical analysis, showed that crack bridging provided the major contribution towards the improvement in fracture toughness. Debonding between the MWCNTs and the matrix appeared to occur in the matrix, away from the actual interface. However, the absence of significant pull-out of broken sections of the MWCNTs during fracture, due to failure of the bridging CNTs being predominantly at the crack plane, indicates that further toughening may be available if this mechanism can be activated.     

Characterization and mechanical testing of alumina-based nanocomposites reinforced with niobium and/or carbon nanotubes fabricated by spark plasma sintering

Alumina-based nanocomposites reinforced with niobium and/or carbon nanotubes (CNT) were fabricated by advanced powder processing techniques and consolidated by spark plasma sintering. Raman spectroscopy revealed that single-walled carbon nanotubes (SWCNT) begin to break down at sintering temperatures >1150 °C. Nuclear magnetic resonance showed that, although thermodynamically unlikely, no Al₄C₃ formed in the CNT-alumina nanocomposites, such that the nanocomposite can be considered as purely a physical mixture with no chemical bond formed between the nanotubes and ceramic matrix. In addition, in situ single-edge notched bend tests were conducted on niobium and/or CNT-reinforced alumina nanocomposites to assess their toughness. Despite the absence of subcritical crack growth, average fracture toughness values of 6.1 and 3.3 MPa m^1/2 were measured for 10 vol.% Nb and 10 vol.% Nb-5 vol.% SWCNT-alumina, respectively. Corresponding tests for the alumina nanocomposites containing 5 vol.% SWCNT, 10 vol.% SWCNT, 5 vol.% double-walled-CNT and 10 vol.% Nb yielded average fracture toughnesses of 3.0, 2.8, 3.3 and 4.0 MPa m^1/2, respectively. It appears that the reason for not observing improvement in fracture toughness of CNT-reinforced samples is because of either damage to CNTs or possibly non-optimal interfacial bonding between CNT-alumina.     

Microstructure and properties of W-ZrC composites prepared by the displacive compensation of porosity (DCP) method

Tungsten-zirconium carbide composites were fabricated at different temperatures by the displacive compensation of porosity (DCP) method, the microstructure, mechanical properties, and ablation resistance were investigated. It was found that no WC phase was left in the composites prepared at 1400 °C, and a few residual W₂C particles were surrounded in W product. Microstructure analyses revealed that zirconium atoms diffused into tungsten carbide to form ZrC and W₂Zr besides carbon diffused into the Zr₂Cu melt. Composites fabricated at 1400 °C had a flexural strength of 356.7 ± 15.2 MPa, an elastic modulus of 193.7 ± 9.8 GPa, a fracture toughness of 7.0 ± 0.7 MPa m^1/2, and a hardness of 13.6 ± 0.7 GPa. After ablated by an oxyacetylene flame for 30 s, the higher temperature prepared composites had a better ablation resistance, the linear ablation rate was 0.0033 ± 0.0004 mm/s, and the mass ablation rate was 0.0012 ± 0.0001 g/s.     

A new TiB2 + CrSi2 composite – Densification,characterization and oxidation studies

A new composite of TiB₂ with CrSi₂ has been prepared with excellent oxidation resistance. Dense composite pellets were fabricated by hot pressing of powder mixtures. Microstructural characterization was carried out by XRD and SEM with EDAX. Mechanical and physical properties were evaluated. Extensive oxidation studies were also carried out. A near theoretical density (99.9% TD) was obtained with a small addition of 2.5 wt.% CrSi₂ by hot pressing at 1700 °C under a pressure of 28 MPa for 1 h. The microstructure of the composite revealed three distinct phases, (a) dark grey matrix of TiB₂, (b) black phase – rich in Si and (c) white phase – Cr laden TiB₂. Hardness and fracture toughness were measured as 29 ± 2 GPa and 5.97 ± 0.61 MPa m^1/2, respectively. Crack branching, deflection and bridging mechanisms were responsible for the higher fracture toughness. With increase in CrSi₂ content, density, hardness and fracture toughness values of the composite decreased. Thermo gravimetric studies revealed the start of oxidation of the composite at 600 °C in O₂ atmosphere. Isothermal oxidation of these composites showed better oxidation resistance by formation of a protective oxide layer. TiO₂, Cr₂O₃ and SiO₂ phases were identified on the oxidized surface. Effects of CrSi₂ content, temperature and duration of oxidation on the oxide layer formation are reported. Activation energy of the composite was calculated as ∼110 kJ/mol using Arrhenius equation. Diffusion controlled mechanism of oxidation was observed in all the composites.     

An evaluation of Al2O3-ZrO2 composites produced by coprecipitation method

The objective of this work is to produce Al₂O₃-ZrO₂ composite from nano-sized powders processed by coprecipitation method. Al₂O₃ and mixture of Al₂O₃ + 10 wt.% ZrO₂ precipitated successfully by chemical route from aluminum sulfate and zirconium sulfate were pressed under uniaxial compression of 170 MPa and sintered at 1600 °C for 1 h. SEM investigations revealed that, pure alumina sample has a microstructure with coarse grains which anisotropically grown up to 30-40 μm in size. In alumina-zirconia composite, the structure consists of very fine equiaxed grains of typically 2 μm in which zirconia precipitates were uniformly dispersed. By adding zirconia to alumina, hardness and indentation fracture toughness were increased from 11.6 GPa to 16.8 GPa and from 3.2 MPa m^1/2 to 4.9 MPa m^1/2, respectively. Improvement in fracture toughness was attributed to bridging effects of zirconia particles as well as transformation toughening.     

Pseudocapacitive performance of hybrid manganese oxide films with multiwalled-CNT additions

In the present study, hybrid manganese oxide films with additions of multiwalled carbon nanotubes (MWCNTs) were prepared by sol-gel process. Manganese acetate was used as the precursors and MWCNTs were added during the process. The effects of MWCNT addition and post heat treatment on the material characteristics and pseudocapacitive performance of the hybrid MWCNT/MnO_x films were investigated. Experimental results showed that manganese oxide was composed of Mn₃O₄ (minor) and Mn₂O₃ (major) phases after heat treatment. MWCNTs served as the template for the growth of manganese oxide films. Among the hybrid films prepared in the present study, manganese oxide films with 0.05 wt.% MWCNT addition heat treated at 350 °C exhibited the best electrochemical performance. The maximum specific capacitance was 340.3 F/g and retained 280.8 F/g (82.5%) after 1000 CV tests. With the addition of MWCNTs, not only the specific capacitance increased but also the reliability improved.     

Synthesis, microstructure and mechanical properties of reaction-infiltrated TiB2-SiC-Si composites

TiB₂-C preforms formed with different compositions and processing parameters were reactively infiltrated by Si melts at 1450 °C to fabricate TiB₂-SiC-Si composites. Phase constituent and microstructure of these composites were analyzed by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The resulting composites are generally composed of TiB₂ and reaction-formed β-SiC major phases, together with a quantity of residual Si. Unreacted carbon is detected in the samples with a starting composition of 2TiB₂ + 1C formed at higher pressure and in all of the ones at the composition of 1TiB₂ + 1C. The distribution of these phases is fairly homogeneous in microstructure. TiB₂-SiC-Si composites show good mechanical properties, with representative values of 19.9 GPa in hardness, 395 GPa in elastic modulus, 3.5 MPa m^1/2 in fracture toughness and 604 MPa in bending strength. The primary toughening and strengthening mechanism is attributed to the crack deflection of TiB₂ particles.     

Optimization of processing conditions and characterization investigations of ceramic injection molded and sintered ZrO2/WC composites

In this investigation, 3 mol% Y₂O₃ stabilized ZrO₂-based composites reinforced with 10 vol.%, 20 vol.% and 40 vol.% WC (named as 3Y-TZP/10WC, 3Y-TZP/20WC and 3Y-TZP/40WC) were fabricated by using injection molding and sintering. Mechanical properties of these composites varied due to WC addition and dwelling time. Density, strength and toughness decreased with shorter dwelling time and increasing WC content however a significant enhancement in fracture toughness was obtained by 3Y-TZP/20WC composite which had 9.2 MPa m^1/2 toughness. Severe unlubricated wear tests which were performed under 55 N normal load and 45 km sliding distance showed that 3Y-TZP/20WC composite had the lowest wear rate and wear volume values which are 2 × 10⁻⁸ mm³/(N m⁻¹) and 0.05 mm³, respectively.     

The effect of the carbon nanotubes surface oxidation on the morphology and properties of poly(N-vinylcarbazole) coated multi-walled carbon nanotube nanocables

This article describes the effect of carbon nanotubes (CNTs) outer surface oxidation on the morphology and properties of poly(N-vinylcarbazole) (PNVC)-coated individual multi-walled CNT (MWCNT) nanocables. Surface oxidation of MWCNTs has been carried out by refluxing MWCNTs with 5 M nitric acid (HNO₃) at 80 °C for 1 h. The PNVC-coated MWCNT nanocables are synthesized by in situ solid-state polymerization of N-vinylcarbazole monomers in the presence of oxidised MWCNTs (o-MWCNTs) at an elevated temperature. The PNVC-coated MWCNT nanocables are characterized by Fourier-transform infrared spectroscopy, X-ray photoelectron spectroscopy, field-emission scanning and transmission electron microscopes, photo-luminescence spectroscopy, and direct-current conductivity measurements. Results show that the uniform nanolayer coating of PNVC decreases the inherent bulk conductivity of MWCNTs, but significantly increases the optical properties of MWCNTs.     

Enhanced electrochemical performances of multi-walled carbon nanotubes modified Li3V2(PO4)3/C cathode material for lithium-ion batteries

The multi-walled carbon nanotubes (MWCNTs) modified Li₃V₂(PO₄)₃/C composite is synthesized by polyvinyl alcohol (PVA) based carbon-thermal reduction method using MWCNTs as a highly conductive agent. PVA mainly supplies a reductive atmosphere to reduce V⁵⁺ and provides a network of carbon to inhibit the aggregation of Li₃V₂(PO₄)₃ particles. The amorphous carbon coating and MWCNTs co-modified composite shows excellent high-rate lithium intercalation/deintercalation property and cycling performance between 3.0 and 4.3 V. The discharge capacities of 131.7 and 122.9 mAh g⁻¹ are obtained at rates of 1 C and 10 C, respectively, for the Li₃V₂(PO₄)₃/(C + MWCNTs). These improvements are attributed to the valid conducting networks of C + MWCNTs and the reduced Li₃V₂(PO₄)₃ particle size by the network carbon from the pyrolysis of PVA.     

The effect of sintering temperature on some properties of Cu-SiC composite

Copper matrix composites reinforced with 1 wt.%, 2 wt.%, 3 wt.% and 5 wt.% SiC particles were fabricated by powder metallurgy method. Cu and Cu-SiC powder mixtures were compacted with a compressive force of 280 MPa and sintered in an open atmospheric furnace at 900-950 °C for 2 h. Within the furnace compacted samples were embedding into the graphite powder. The presence of Cu and SiC components in composites was verified by XRD analysis. Optical and SEM studies showed that Cu-SiC composites have a uniform microstructure in which silicon carbide particles are distributed uniformly in the copper matrix. The results of the study on mechanical and electrical conductivity properties of Cu-SiC composites indicated that with increasing SiC content (wt.%), hardness increased, but relative density and electrical conductivity decreased. The highest electrical conductivity of 98.8% IACS and relative density of 98.2% were obtained for the Cu-1 wt.%SiC composite sintered at 900 °C and this temperature was defined as the optimum sintering temperature.     

Properties and fast low-temperature consolidation of nanocrystalline Ni-ZrO2 composites by high-frequency induction heated sintering

Nanopowders of Ni and ZrO₂ (11 nm and 90 nm, respectively) were synthesized from NiO and Zr by high energy ball milling. A highly dense nanostructured 2Ni-ZrO₂ composite was consolidated at low temperature by high-frequency induction heat sintering within 2 min of the mechanical synthesis of the powders (Ni-ZrO₂) with horizontal milled NiO + Zr powders under 500 MPa pressure. This process allows very quick densification to near theoretical density and prohibits grain growth in nano-structured materials. The grain sizes of Ni and ZrO₂ in the composite were calculated. Finally, the average hardness and fracture toughness values of nanostructured 2Ni-ZrO₂ composites were investigated.     

Bulk WC-Al2O3 composites prepared by spark plasma sintering

WC and WC-Al₂O₃ materials without metallic binder addition were densified by spark plasma sintering in the range of 1800-1900 °C. The densification behavior, phase constitution, microstructure and mechanical properties of pure WC and WC-Al₂O₃ composite were investigated. The addition of Al₂O₃ facilitates sintering and increases the fracture toughness of the composites to a certain extent. An interesting phenomenon is found that a proper content of Al₂O₃ additive helps to limit the formation of W₂C phase in sintered WC materials. The pure WC specimen possesses a hardness (HV₁₀) of 25.71 GPa, fracture toughness of 4.54 MPa·m^1/2, and transverse fracture strength of 862 MPa, while those of WC-6.8 vol.% Al₂O₃ composites are 24.48 GPa, 6.01 MPa·m^1/2, and 1245 MPa respectively. The higher fracture toughness and transverse fracture strength of WC-6.8 vol.% Al₂O₃ are thought to result from the reduction of W₂C phase, the crack-bridging by Al₂O₃ particles and the local change in fracture mode from intergranular to transgranular.     

An investigation on corrosion behaviour of pressure infiltrated Al-Mg alloy/SiCp composites

In this study, effect of Mg alloying addition (2-8 wt.%) on corrosion behaviour of Al matrix composites, in 3.5 wt.% NaCl environment, has been investigated. Composites were produced by pressure infiltration technique at 750 °C and had a SiC particle (SiC_p) volume fraction of ∼60%. Results were evaluated by using potentiodynamic polarisation measurements, immersion tests, SEM, EDS and XRD analysis. Compared to the pure Al matrix, mass loss of the composites decreased with increasing Mg content. Experimental results revealed that intermetallics as a result of reaction between Al-Mg alloy and SiC particle has beneficial effect on corrosion resistance of the composites due to interruption of the continuity of the matrix channels within the pressure infiltrated composites.     

Investigations on synthesis of ZrB2 and development of new composites with HfB2 and TiSi2

This paper presents the results of experimental investigations carried out on the synthesis of pure ZrB₂ by boron carbide reduction of ZrO₂ and densification with the addition of HfB₂ and TiSi₂. Process parameters and charge composition were optimized to obtain pure ZrB₂ powder. Monolithic ZrB₂ was hot pressed to full density and characterized. Effects of HfB₂ and TiSi₂ addition on densification and properties of ZrB₂ composites were studied. Four compositions namely monolithic ZrB₂, ZrB₂ + 10% TiSi₂, ZrB₂ + 10% TiSi₂ + 10% HfB₂ and ZrB₂ + 10% TiSi₂ + 20% HfB₂ were prepared by hot pressing. Near theoretical density (99.8%) was obtained in the case of monolithic ZrB₂ by hot pressing at 1850 °C and 35 MPa. Addition of 10 wt.% TiSi₂ resulted in an equally high density of 98.9% at a lower temperature (1650 °C) and pressure (20 MPa). Similar densities were obtained for ZrB₂ + HfB₂ mixtures also with TiSi₂ under similar conditions. The hardness of monolithic ZrB₂ was measured as 23.95 GPa which decreased to 19.45 GPa on addition of 10% TiSi₂. With the addition of 10% HfB₂ to this composition, the hardness increased to 23.08 GPa, close to that of monolithic ZrB₂. Increase of HfB₂ content to 20% did not change the hardness value. Fracture toughness of monolithic sample was measured as 3.31 MPa m^1/2, which increased to 6.36 MPa m^1/2 on addition of 10% TiSi₂. With 10% HfB₂ addition the value of K_IC was measured as 6.44 MPa m^1/2, which further improved to 6.59 MPa m^1/2 with higher addition of HfB₂ (20%). Fracture surface of the dense bodies was examined by scanning electron microscope. Intergranular fracture was found to be a predominant mode in all the samples. Crack propagation in composites has shown considerable deflection indicating high fracture toughness. An oxidation study of ZrB₂ composites was carried out at 900 °C in air for 64 h. Specific weight gain vs time plot was obtained and the oxidized surface was examined by XRD and SEM. ZrB₂ composites have shown a much better resistance to oxidation as compared to monolithic ZrB₂. A protective glassy layer was seen on the oxidized surfaces of the composites.     

The relationship between microstructure and fracture toughness of zirconia toughened alumina (ZTA) added with MgO and CeO2

The aim of this research is to investigate the mode of crack propagation in zirconia toughened alumina (ZTA) added with MgO and CeO₂, respectively. The mode of crack refers to the toughening mechanism of the materials. Different ZTA compositions containing MgO and CeO₂ as sintering additives were prepared using pressureless sintering at 1600 °C. Each sample was subjected to Vickers indentation with 294 N load and the cracks that propagated were observed with SEM. The ZTA with an addition of 0.7 wt.% MgO showed a crack deflection with a fracture toughness value of 6.19 ± 0.26 MPa · √m. On the other hand, the ZTA with CeO₂ addition of 0.5 to 7 wt.% showed both crack bridging and deflection, and produced 5.78 ± 0.16 MPa · √m to 6.59 ± 0.23 MPa · √m fracture toughness values, respectively. The fracture toughness of the ZTA–MgO–CeO₂ compositions is higher due to crack bridging and crack deflection. The toughening mechanisms of crack deflection and bridging hinder crack propagation since more energy is required to make the crack propagate. However, the formation of CeAl₁₁O₁₈ phase was observed; this consequently decreases the hardness and fracture toughness of the ZTA–MgO–CeO₂ compositions.     

Microstructures and mechanical properties of the in situ TiB-Ti metal-matrix composites synthesized by spark plasma sintering process

In situ synthesized TiB reinforced titanium matrix composites have been synthesized by spark plasma sintering (SPS) process at 950-1250 °C, using mixtures of 15 wt% TiB₂ and 85 wt% Ti powders. The effects of the sintering temperature on densification behavior and mechanical properties of the TiB-Ti composites were investigated. The results indicated that with rising sintering temperatures, relative densities of the composites increase obviously, while the in situ TiB whiskers grow rapidly. As a result, bending strength of the TiB-Ti composites increases slowly at the combined actions of the factors referred above. Fracture toughness of the composites is improved remarkably due to the large volume fraction of Ti matrix, the crack deflection, pull-out and the micro-fracture of the needle-shaped TiB grains. The results also suggested that TiB-Ti composite sintered at 1250 °C by SPS process exhibits the highest relative density of 99.6% along with bending strength of 1161 MPa and fracture toughness of 13.5 MPa m^1/2.     

Influence of SiC particles addition on the corrosion behavior of 2014 Al-Cu alloy in 3.5% NaCl solution

The influence of silicon carbide particles (SiC_p) addition on the corrosion behavior of Al-Cu alloy (2014) was evaluated in 3.5% NaCl solution at 30 °C using microstrucural and electrochemical measurements. Addition of 10 wt.% SiC_p to the base alloy is found to increase its corrosion resistance considerably. Incorporation of SiC_p beyond this proportion leads to an increase in corrosion rate of the synthesized composites. Addition of 25 wt.% SiC_p to base alloy decreases corrosion resistances considerably. Microstructural studies reveal the agglomeration of SiC particles in the composites. This results an increase of corrosion reaction with the increase of SiC particles in the composites. EIS measurement indicates the occurrence of adsorption/diffusion phenomena at the interfaces of the composites that ultimately initiate the localized or pitting corrosion.