Hard and tough carbon nanotube-reinforced zirconia-toughened alumina composites prepared by spark plasma sintering

It is demonstrated that 0.1 wt% of multi-walled carbon nanotubes (MWCNTs) or single-walled carbon nanotubes (SWCNTs) added to zirconia toughened alumina (ZTA) composites is enough to obtain high hardness and fracture toughness at indentation loads of 1, 5, and 10 kg. ZTA composites with 0.01 and 0.1 wt% of MWCNTs or SWCNTs were densified by spark plasma sintering (SPS) at 1520 °C resulting in a higher hardness and comparable fracture toughness to the ZTA matrix material. The observed toughening mechanisms include crack deflection, pullout of CNTs as well as bridged cracks leading to improved fracture toughness without evidence of transformation toughening of the ZrO₂ phase. Scanning electron microscopy showed that MWCNTs rupture by a sword-in-sheath mechanism in the tensile direction contributing to an additional increase in fracture toughness.     

Development and evaluation of Al2O3–ZrO2 composite processed by digital light 3D printing

Digital Light Processing (DLP) is a promising approach to fabricate delicate ceramic components with high-fidelity structural features. In this work, the alumina and zirconia/alumina ceramic suspensions with low viscosity and high solid loading (40 vol%) were prepared specifically for DLP 3D printing. After debinding and sintering, the final parts were obtained without any defects. The surface morphologies and mechanical properties of alumina (Al₂O₃) and zirconia toughened alumina (ZTA) composites were investigated and the results showed that the final parts exhibited high relative densities and good interlayer combination at the sintering temperature of 1600 °C. Comparing with the Al₂O₃, the ZTA composites exhibited significantly enhanced density (99.4%), bending strength (516.7 MPa) and indentation fracture toughness (7.76 MPa m^1/2).     

Fabrication and mechanical properties of Al2O3–TiC ceramic composites synergistically reinforced with multi-walled carbon nanotubes and graphene nanoplates

In this study, Al₂O₃–TiC composites synergistically reinforced with multi-walled carbon nanotubes (MWCNTs) and graphene nanoplates (GNPs) were prepared via spark plasma sintering (SPS). The effects of the MWCNT and GNP contents on the phase composition, mechanical properties, fracture mode, and toughening mechanism of the composites were systematically investigated. The experimental results indicated that the composite grains became more refined with the addition of MWCNTs and GNPs. The nanocomposites presented high compactness and excellent mechanical properties. The composite with 0.8 wt% MWCNTs and 0.2 wt% GNPs presented the best properties of all analysed specimens, and its relative density, hardness, and fracture toughness were 97.3%, 18.38 ± 0.6 GPa, and 9.40 ± 1.6 MPa m^1/2, respectively. The crack deflection, bridging, branching, and drawing effects of MWCNTs and GNPs were the main toughening mechanisms of Al₂O₃–TiC composites synergistically reinforced with MWCNTs and GNPs.     

Structural properties and mechanical behavior of SWCNTs and MWCNTs reinforced Al2O3 fabricated by spark plasma sintering

Carbon nanotubes due to their structural and mechanical properties are good candidates as the second phase to improve the mechanical properties of alumina-based ceramics. In the present study, the effects of single wall and multi-wall carbon nanotubes on structural and mechanical properties of alumina were investigated. SWCNTs and MWCNTs were dispersed in alumina powder via a conventional method using 1 wt % PVA water solution as media. Sintering process for two different composite powders, alumina-2 wt. % SWCNTs and alumina 2 wt % MWCNTs was performed by spark plasma sintering technique at 1500 °C and 20 MPa for 10 min. Results showed that the presence of CNTs in alumina caused a considerable amount of porosity in final bodies. SEM images of fracture surfaces revealed the agglomeration of SWCNTs which played a dominant role in the deterioration of mechanical properties. MWCNTs reinforced alumina obtained higher Vickers hardness and bending strength values (12.91 GPa and 291 MPa, respectively) compared to that of SWCNTs (9.18 GPa and 276 MPa, respectively), due to sever agglomerate of SWCNTs throughout sintered composites. Typical load-displacement (P/h) curves were obtained from bending strength test and discussed. It was concluded that the addition of MWCNTs to alumina represented better densification and mechanical properties compared to SWCNTs.     

Toughening of zirconia/alumina composites by the addition of graphene platelets

A study on graphene platelet/zirconia-toughened alumina (GPL/ZTA) composites was carried out to evaluate the potential of the new structural materials. GPL–ZrO₂–Al₂O₃ powders were obtained by ball milling of graphene platelets and alumina powders using yttria stabilized ZrO₂ balls. Samples were sintered at different temperatures using spark plasma sintering. Fracture toughness was determined by the single-edge notched beam method. The results show that the GPLs are uniformly distributed in the ceramic matrix and have survived high temperature sintering processes. Several sintering experiments were carried out. It is found that at 1550 °C, GPL/ZTA composites were obtained with nearly full density, maximum hardness and fracture toughness. A 40% increase in fracture toughness in the ZTA composite has been achieved by adding graphene platelets. The toughening mechanisms, such as pull out, bridging and crack deflection, were observed and are discussed.     

Carbon nanotube/polymer nanocomposites: A study on mechanical integrity through nanoindentation

Carbon nanotubes (CNTs) are under intense investigation in materials science owing to their potential for modifying the mechanical proprieties of their composites. In this work, nanomechanical and nanotribological properties of polymer composites, reinforced with multiwall carbon nanotubes (MWCNTs) and single wall carbon nanotubes (SWCNTs), have been studied using the nanoindentation and nanoscratch technique. In particular, three different epoxy resins reinforced using several percentage of two different types of MWCNTs have been studied (range 0–7 wt%). Another resin was reinforced using MWCNTs (range 0–2.5 wt%) and SWCNTs (range 0–5 wt%) as fillers. Hardness and elastic modulus using nanoindenter instrument have been evaluated, while the coefficient of friction of the nanocomposites is obtained using nanoscratch. The results show an evident dependence with the percentage of CNTs. For all types of resins, an optimum in nanomechanical properties is found at intermediate levels of CNTs filling. POLYM. COMPOS., 36:1432–1446, 2015. © 2014 Society of Plastics Engineers     

Grain growth kinetics in microwave sintered graphene platelets reinforced ZrO2/Al2O3 composites

The grain growth kinetics and mechanical properties of graphene platelets(GPLs) reinforced ZrO₂/Al₂O₃(ZTA) composites prepared by microwave sintering were investigated. The calculated grain growth kinetics exponent n indicated that the GPLs could accelerate the process of the Al₂O₃ columnar crystal growth. And the grain growth activation energy of the Al₂O₃ columnar crystal indicated that the grain growth activation energy of the GPLs doped ZTA composites is much higher than those of pure Al₂O₃ and ZTA in microwave sintering. The optimal mechanical properties were achieved with 0.4?vol% GPLs, whose relative density, Vickers hardness and fracture toughness were 98.76%, 18.10?GPa and 8.86?MPa?m^1/2, respectively. The toughening mechanisms were crack deflection, bridging, branching and pull-out of GPLs. The results suggested that GPLs-doped are good for the Al₂O₃ columnar crystal growth in the ZTA ceramic and have a potentially improvement for the fracture toughness of the ceramics.     

Mechanical properties of graphene platelet-reinforced alumina ceramic composites

Alumina (Al₂O₃) ceramic composites reinforced with graphene platelets (GPLs) were prepared using Spark Plasma Sintering. The effects of GPLs on the microstructure and mechanical properties of the Al₂O₃ based ceramic composites were investigated. The results show that GPLs are well dispersed in the ceramic matrix. However, overlapping of GPLs and porosity within ceramics are observed. The flexural strength and fracture toughness of the GPL-reinforced Al₂O₃ ceramic composites are significantly higher than that of monolithic Al₂O₃ samples. A 30.75% increase in flexural strength and a 27.20% increase in fracture toughness for the Al₂O₃ceramic composites have been achieved by adding GPLs. The toughening mechanisms, such as pull-out and crack deflection induced by GPLs are observed and discussed.     

Mechanical properties and electrical conductivity in a carbon nanotube reinforced silicon nitride composite

The influence of carbon nanotubes (CNTs) addition on basic mechanical, thermal and electrical properties of the multiwall carbon nanotube (MWCNT) reinforced silicon nitride composites has been investigated. Silicon nitride based composites with different amounts (1 or 3 wt%) of carbon nanotubes have been prepared by hot isostatic pressing. The fracture toughness was measured by indentation fracture and indentation strength methods and the thermal shock resistance by indentation method. The hardness values decreased from 16.2 to 10.1 GPa and the fracture toughness slightly decreased by CNTs addition from 6.3 to 5.9 MPa m^1/2. The addition of 1 wt% CNTs enhanced the thermal shock resistance of the composite, however by the increased CNTs addition to 3 wt% the thermal shock resistance decreased. The electrical conductivity was significantly improved by CNTs addition (2 S/m in 3% Si₃N₄/CNT nanocomposite).     

Mechanical properties of SiCp/Al2O3 ceramic matrix composites prepared by directed oxidation of an aluminum alloy

Silicon carbide particulate reinforced alumina matrix composites were fabricated using DIrected Metal OXidation (DIMOX) process. Continuous oxidation of an Al-Si-Mg-Zn alloy with appropriate dopants along with a preform of silicon carbide has led to the formation of alumina matrix surrounding silicon carbide particulates. SiC_p/Al₂O₃ ceramic matrix composites fabricated by the DIMOX process, possess enhanced mechanical properties such as flexural strength, fracture toughness and wear resistance, all at an affordable cost of fabrication. SiC_p/Al₂O₃ matrix composites were investigated for mechanical properties such as flexural strength, fracture toughness and hardness; the composite specimens were evaluated using standard procedures recommended by the ASTM. The SiC_p/Al₂O₃ ceramic matrix composites with SiC volume fractions from 0.35 to 0.43 were found to possess average bend strength in range 158-230 MPa and fracture toughness was found to be in range of 5.61-4.01 MPa√m. The specimen fractured under three-point loading as observed under scanning electron microscope was found to fail in brittle manner being the dominant mode. Further the composites were found to possess lower levels of porosity, among those prepared by DIMOX process.     

Effect of Al2O3 particle size on preparation and properties of ZTA ceramics formed by gelcasting

Zirconia-toughened alumina (ZTA) ceramics were prepared using three different kinds of Al₂O₃ powders (marked PW-A average particle size: 7.53 μm, marked PW-B average particle size: 1.76 μm, marked PW-C average particle size: 0.61 μm) by gelcasting. Effect of Al₂O₃ particle size on zeta potential, dispersant dosage and solid volume fractions of ZTA suspensions as well as the mechanical properties of ZTA green bodies and ceramics were investigated. The optimum dosages of dispersant for ZTA suspensions prepared by PW-A, PW-B and PW-C are 0.4 wt%, 0.5 wt% and 0.7 wt%, respectively. The highest solid volume fractions of ZTA suspensions can reach 62 vol% (SP-A), 60 vol% (SP-B) and 52 vol% (SP-C), respectively. The green bodies show a bending strength as high as 20 MPa, which can meet the requirement of machining. The Al₂O₃ powder with fine particle size is beneficial to the improvement of mechanical properties. The ZTA ceramics prepared by PW-B Al₂O₃ powder show the highest bending strength (680 MPa) and toughness (7.49 MPa m^1/2).     

Nanoplates forced alignment of multi-walled carbon nanotubes in alumina composite with high strength and toughness

Although the strengthening and toughening effects on ceramic composites are expected to be maximized by alignment of multi-walled carbon nanotubes (MWCNTs) in matrices, this concept has been rarely realized in practice due to the lack of convenient processing strategy. Here, the alignment of MWCNTs in alumina composite can be readily obtained by using α-Al₂O₃ nanoplates as raw powder. With the assistance of vacuum filtration and pressure in sintering, the highly aligned MWCNTs in alumina matrix are formed in in-plane direction. Accordingly, the strength and toughness in 1.5 wt% MWCNTs/alumina composite are improved by 58 % and 66 % with respect to monolithic alumina, respectively. Transmission electron microscopy observation reveals that the MWCNTs under great compressive residual stress are mainly embedded inside the grains, leading to much stronger grain boundaries. Meanwhile, the toughening effect is mainly attributed to the highly energy dissipating bridging and pullout, owing to the very effective load transfer.     

Evaluation of mechanical reliability of zirconia-toughened alumina composites for dental implants

Zirconia-toughened alumina composites containing 0–30 vol% of 3Y-TZP were fabricated by sintering at 1600 °C for 2 h in air. The effect of the 3Y-TZP content on the mechanical properties and microstructure of the alumina ceramics was investigated. The fracture toughness and biaxial flexural strength increased as the 3Y-TZP content increased. The Young's modulus decreased with 3Y-TZP content according to the rule of mixture, while the hardness showed the contrary tendency. The Weibull modulus of the Al₂O₃ with 20 vol% 3Y-TZP composite is higher than that of alumina. The residual hoop compressive stress developed in ZTA ceramic composites probably accounts for the enhancement of strength and fracture toughness, as well as for the higher tendency of crack deflection. No monoclinic phase and strength degradation were found after low temperature degradation (LTD) testing. The excellent LTD resistance can be explained by the increased constraining force on zirconia embedded in alumina matrix.     

Mechanical and functional properties of Al2O3–ZrO2–MWCNTs nanocomposites

Multi-walled carbon nanotubes (MWCNTs) are often reported as additives improving mechanical and functional properties of ceramic composites. However, despite tremendous efforts in the field in the past 20 years, the results are still inconclusive. This paper studies room temperature properties of the composites with polycrystalline alumina matrix reinforced with 0.5–2 vol.% MWCNTs (composites AC) and zirconia toughened alumina with 5 vol.% of yttria partially stabilised zirconia (3Y-PSZ) containing 0.5–2 vol.% of MWCNTs (composites AZC). Dense composites were prepared through wet mixing of the respective powders with functionalised MWCNTs, followed by freeze granulation, and hot-pressing of granulated powders. Room temperature bending strength, Young's modulus, indentation fracture toughness, thermal and electrical conductivity of the composites were studied, and related to their composition and microstructure. Slight increase of Young's modulus, indentation fracture toughness, bending strength, and thermal conductivity was observed at the MWCNTs contents ≤1 vol.%. At higher MWCNTs contents the properties were impaired by agglomeration of the MWCNTs. The DC electrical conductivity increased with increasing volume fraction of the MWCNTs.     

Fabrication and characterization of SiC-ZTA ceramic composites by hot pressing

Al₂O₃/ZrO₂/SiC ceramic composites with different SiC contens have been prepared by hot pressuring. The effect of SiC content on the microstructure and mechanical properties of composites have been studied. The results show that SiC has obvious grain refinement effect on ZTA ceramics and change the fracture mode of the matrix from intergranular fracture to transgranular fracture. Simultaneously, it has been found that the mechanical properties of the material are significantly enhanced in comparison with ZTA matrix. The highest strength is acquired at 10% SiC content, the flexural strength and toughness are obtained when the SiC content is 15 vol%, and the values are 18.86 GPa, 1262 MPa and 6.13 MPa m^1/2, respectively. The mechanisms of hardening, strengthening and toughening have been discussed.     

Effect of functionalized MWCNTs on the thermo-mechanical properties of poly(5-ethylidene-2-norbornene) composites produced by ring-opening metathesis polymerization

Functionalized multiwalled carbon nanotubes (MWCNTs) reinforced poly(5-ethylidene-2-norbornene (ENB)) composites have been fabricated via ring-opening metathesis polymerization. Verification of covalent bond formation between the functionalized carbon nanotubes and the polyENB matrix was demonstrated by solvent exposure followed by thermal gravimetry. The tensile toughness of the composites increased by 300% with dramatic morphological changes on the resulting fracture surfaces when just 0.8 wt% norbornene-functionalized MWCNTs (f-MWCNTs) were added to the polymer. A slight increase of glass-transition temperature was observed by dynamic mechanical analysis compared to a decreased value with unfunctionalized MWCNTs.     

Microstructure and strengthening behavior in high content SiC nanowires reinforced SiC composites

In this study, the high-content SiC_nw reinforced SiC ceramic matrix composites (SiC_nw/SiC CMC) were successfully fabricated by hot pressing β-SiC and sintering additive (Al₂O₃-Y₂O₃) with boron nitride interphase modification SiC_nw. The effects of sintering additive content and mass fraction (5–25 wt%) of SiC_nw on the density, microstructure, and mechanical properties of the composites were investigated. The results showed that with the increase of sintering additives from 10 wt% to 12 wt%, the relative density of the SiC_nw/SiC CMC increased from 97.3% to 98.9%, attributed to the generated Y₃Al₅O₁₂ (YAG) liquid phase from the Al₂O₃-Y₂O₃ that promotes the rearrangement and migration of SiC grains. The comprehensive performance of the obtained composite with 15 wt% SiC_nw possessed the optimal flexural strength and fracture toughness of 524 ± 30.24 MPa and 12.39 ± 0.49 MPa·m^1/2, respectively. Besides, the fracture mode of the composites with 25 wt% SiC_nw content revealed a pseudo-plastic fracture behavior. It concludes that the 25 wt% SiC_nw/SiC CMC was toughened by the fiber pull-outs, debonding, bridging, and crack deflection that can consume plenty of fracture energy. The strategy of SiC nanowires worked as a main bearing phase for the fabrication of SiC/SiC CMC providing critical information for understanding the mechanical behavior of high toughness and high strength SiC nanoceramic matrix composites.     

Addition of Al–Ti–B master alloys to improve the performances of alumina matrix ceramic materials

In the present work, a new technique to improve the performances of alumina matrix ceramic materials is presented, in which Al, Al₃Ti and TiB₂ are incorporated into alumina matrix ceramic materials in the form of Al–Ti–B master alloys. Composites of Al₂O₃/TiB₂/AlN/TiN are fabricated by the technology of transient liquid phase sintering, during which new phases such as AlN and TiN are produced by the chemical reactions taking place among Al, Ti and N₂ (the protective atmosphere). The densification rate of the composites as a function of Al–Ti–B volume content is discussed. The fundamental properties of the composites such as hardness, fracture toughness and bending strength are examined. The relations of volume content of Al–Ti–B master alloys and mechanical properties of alumina matrix ceramic materials are analyzed. The effects of fracture mechanism on mechanical properties of the composites are researched together with the refining performances of Al–Ti–B master alloys.     

Determination of mechanical properties of Al2O3/Y-TZP ceramic composites: Influence of testing method and residual stresses

A series of Al₂O₃/Y₂O₃-stabilized zirconia (Y-TZP) ceramic composites with different zirconia contents (5 and 40 vol% Y-TZP) and fabricated by different green processing techniques (a novel tape casting and conventional slip casting) were studied. The microstructure and mechanical properties of the composites were investigated systematically, by means of scanning electron microscopy, Vickers indentation, depth-sensing nanoindentation, and single-edge laser-notched beam (SELNB) techniques. The indentation fracture method was found to be unsuitable for fracture toughness determination in this work. Reliable values of fracture toughness were obtained by the SELNB method with an almost atomically sharp laser-machined initial notch. The microstructure and mechanical properties of the ceramic composites mainly depended on the Y-TZP content. No significant differences were induced by the choice of green processing technique. The contribution of residual stresses to fracture toughness in Al₂O₃/Y-TZP ceramic composites was investigated. To this end, a theoretical model was applied to estimate the increase in fracture toughness due to the measured residual stresses in the samples. It was found that in this case, residual stresses were not the main factor responsible for the toughening in Al₂O₃/Y-TZP composites.     

Silicon nitride based nanocomposites produced by two different sintering methods

This research explores the use of a variety of carbon nanostructures as reinforcing agents for Si₃N₄ matrix composites. We have chosen highly promising families of carbon materials: multiwall, singlewall carbon nanotubes (MWCNTs, SWCNTs), graphene, carbon black nanograins and graphite micrograins for use as fillers. These materials were dispersed with a concentration of 3 wt% in silicon nitride matrices. A high efficiency attritor mill has also been used for effective dispersion of second phases in the matrix. In the present work the development of sintering processes (hot isostatic pressing (HIP) and spark plasma sintering (SPS)) has been performed to consolidate and tailor the microstructure of Carbon nanotube (CNT)-reinforced silicon nitride-based ceramic composites. The silicon nitride nanocomposite systems retained the mechanical robustness of the original systems. Elastic modulus measurements and micro-indentation investigations of the hardness and fracture toughness have been performed as well as scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X-ray diffraction in order to characterize the composites produced by the two sintering methods.