Grafting of epoxy chains onto graphene oxide for epoxy composites with improved mechanical and thermal properties

Epoxy composites filled with both graphene oxide (GO) and diglycidyl ether of bisphenol-A functionalized GO (DGEBA–f–GO) sheets were prepared at different filler loading levels. The correlations between surface modification, morphology, dispersion/exfoliation and interfacial interaction of sheets and the corresponding mechanical and thermal properties of the composites were systematically investigated. The surface functionalization of DGEBA layer was found to effectively improve the compatibility and dispersion of GO sheets in epoxy matrix. The tensile test indicated that the DGEBA–f–GO/epoxy composites showed higher tensile modulus and strength than either the neat epoxy or the GO/epoxy composites. For epoxy composite with 0.25 wt% DGEBA–f–GO, the tensile modulus and strength increased from 3.15 ± 0.11 to 3.56 ± 0.08 GPa (∼13%) and 52.98 ± 5.82 to 92.94 ± 5.03 MPa (∼75%), respectively, compared to the neat epoxy resin. Furthermore, enhanced quasi-static fracture toughness (K_IC) was measured in case of the surface functionalization. The GO and DGEBA–f–GO at 0.25 wt% loading produced ∼26% and ∼41% improvements in K_IC values of epoxy composites, respectively. Fracture surface analysis revealed improved interfacial interaction between DGEBA–f–GO and matrix. Moreover, increased glass transition temperature and thermal stability of the DGEBA–f–GO/epoxy composites were also observed in the dynamic mechanical properties and thermo-gravimetric analysis compared to those of the GO/epoxy composites.     

Thermal transport phenomena and limitations in heterogeneous polymer composites containing carbon nanotubes and inorganic nanoparticles

An Off-Lattice Monte Carlo model was developed to investigate effective thermal conductivities (K_eff) and thermal transport limitations of polymer composites containing carbon nanotubes (CNTs) and inorganic nanoparticles. The simulation results agree with experimental data for poly(ether ether ketone) (PEEK) with inclusions of CNTs and tungsten disulfide (WS₂) nanoparticles. The developed model can predict the thermal conductivities of multiphase composite systems more accurately than previous models by taking into account interfacial thermal resistance (R_bd) between the nanofillers and the polymer matrix, and the nanofiller orientation and morphology. The effects of (i) R_bd of CNT–PEEK and WS₂–PEEK (0.0232–115.8 × 10⁻⁸ m²K/W), (ii) CNT concentration (0.1–0.5 wt%), (iii) CNT morphology (aspect ratio of 50–450, and diameter of 2–8 nm), and (iv) CNT orientation (parallel, random and perpendicular to the heat flux) on K_eff of a multi-phase composite are quantified. The simulation results show that K_eff of multiphase composites increases when the CNT concentration increases, and when the R_bd of CNT–PEEK and WS₂–PEEK interfaces decrease. The thermal conductivity of composites with CNTs parallel to the heat flux can be enhanced ∼2.7 times relative to that of composites with randomly-dispersed CNTs. CNTs with larger aspect ratio and smaller diameter can significantly improve the thermal conductivity of a multiphase polymer composite.     

Hydrogen-storage properties of MgH2–10Ni–2NaAlH4–2Ti–2CNT milled in a planetary ball mill under H2

A sample with a composition of 84 wt% MgH₂–10 wt% Ni–2 wt% NaAlH₄–2 wt% Ti–2 wt% CNT (named MgH₂–10Ni–2NaAlH₄–2Ti–2CNT) was prepared by milling in a planetary ball mill under H₂. Activation of the sample was not required. At the first cycle, the sample absorbed 3.75 wt% H for 10 min, and 4.17 wt% H for 60 min at 593 K under 12 bar H₂. Reactive mechanical grinding of Mg with Ni, NaAlH₄, Ti, and CNT is thought to create defects on the surface and in the interior of Mg, as well as to reduce Mg particle size.     

The role of titania on the microstructure,biocorrosion and mechanical properties of Mg/HA-based nanocomposites for potential application in bone repair

Bone defects are very challenging in orthopedic practice. The ideal bone grafts should provide mechanical support and enhance the bone healing. Biodegradable magnesium (Mg)–based alloys demonstrate good biocompatibility and osteoconductive properties, which are promising biomaterials for bone substitutes. However, the high rate of their biodegradation in human body environment is still challenging. For this scope, synthesis Mg-based composites with bioceramic additives such as HA and titania (TiO₂) is a routine to solve this problem. The aim of this study was to evaluate the effect of addition TiO₂ nanopowders on the corrosion behavior and mechanical properties of Mg/HA-based nanocomposites fabricated using a milling-pressing-sintering technique for medical applications. The microstructure of Mg/HA/TiO₂ nanocomposites, in vitro degradation and biological properties including in vitro cytocompatibility were investigated. The corrosion resistance of Mg/HA-based nanocomposites was significantly improved by addition 15 wt% of TiO₂ and decrease HA amount to 5 wt% this was inferred from the lower corrosion current; 4.8 µA/cm² versus 285.3 µA/cm² for the Mg/27.5 wt%HA, the higher corrosion potential; −1255.7 versus −1487.3 mV_SCE, the larger polarization resistance; 11.86 versus 0.25 kΩ cm² and the significantly lower corrosion rate; 0.1 versus 4.28 mm/yr. Compressive failure strain significantly increased from 1.7% in Mg/27.5HA to 8.1% in Mg/5HA/15TiO₂ (wt%). The Mg/5HA/15TiO₂ (wt%) nanocomposite possessed high corrosion resistance, cytocompatibility and mechanical properties and can be considered as a promising material for implant applications.     

Effect of suspension stability on bonding strength and electrochemical behavior of electrophoretically deposited HA–YSZ nanostructured composite coatings

In the present study, HA–YSZ nanostructured composites were deposited on Ti–6Al–4 V substrates by electrophoretic deposition of suspensions containing 0, 10, 20 and 40 wt% YSZ. The stability of each suspension was determined by applying response surface methodology, DLVO theory and zeta potential measurement for different YSZ contents and dispersant concentrations. The maximum zeta potential and electromobility of suspended particles was obtained for the suspension with 20 wt% YSZ. The electrophoretic deposition of HA–YSZ nanostructured composites was carried out at a constant voltage of 20 V for 120 s. The deposition kinetics was studied based on a mass-charge correlating approach under ranges of voltage (20–60 V), time (30–300 s) and wt% YSZ (0–40). The as–deposited and sintered HA–YSZ coatings were characterized by SEM, XRD, DSC–TG and FT–IR analyses. The micro-scratch behavior of coated samples indicated the highest critical contact pressures of crack initiation, P_c1 = 4.50 GPa, crack delamination, P_c2 = 5.14 GPa and fracture toughness, K_IC = 0.622 MPa m^1/2 for HA-20 wt% YSZ sample. The results of potentiodynamic polarization measurements showed that the implementation of 20 wt% YSZ could efficiently decrease the corrosion current density and corrosion rate of coated samples, while corrosion potential and linear polarization resistance were increased.     

Physical properties of carbon nanotube sheets drawn from nanotube arrays

We report mechanical, thermal, and electrical properties of novel sheet materials composed of multiwalled carbon nanotubes, drawn from a CNT array. At low loading there is some slippage of CNTs but at higher loading tensile strength σ₀ = 7.9 MPa and Young’s modulus E = 310 MPa. The room-temperature thermal conductivity of the CNT sheet was 2.5 ± 0.5 W m^?1 K^?1, giving a thermal conductivity to density ratio of κ/ρ = 65 W m^?1 K^?1 g^?1 cm³. The heat capacity shows 1D behavior for T > 40 K, and 2D or 3D behavior at lower temperatures. The room-temperature specific heat was 0.83 J g^?1 K^?1. The iV curves above 10 K have Ohmic behavior while the iV curve at T = 2 K is non-Ohmic, and a model to explain both ranges is presented. Negative magnetoresistance was found, increasing in magnitude with decreasing temperature (?15% at T = 2 K and B = 9 T). The tensile strength, Young’s modulus and electrical conductivity of the CNT sheet are low, in comparison with other CNT materials, likely due to defects. Thermal conductivity is dominantly phononic but interfacial resistance between MWCNTs prevents the thermal conductivity from being higher.     

Effect of NiO additive on microstructure,mechanical behavior and electrical properties of 0.2PZN–0.8PZT ceramics

A NiO-added Pb((Zn_1/3Nb_2/3)_0.20(Zr_0.50Ti_0.50)_0.80)O₃ system is prepared and investigated. The results reveal that Ni doping induces a phase transformation from the morphotropic phase boundary to the tetragonal phase side. Above the solubility limit of 0.3 wt% in NiO form, excess Ni ions segregate at the grain boundaries and triple junctions, which facilitate the formation of a liquid phase with excess PbO and lead to remarkable grain growth. The mechanical behavior (Vickers hardness (H_v) and fracture toughness (K_IC)) can be tailored by controlling the content of additive; this is accompanied by a transition in the fracture mode changed from transgranular without NiO additive to intergranular with 1.0 wt% NiO additive. Moreover, the NiO addition weakens the dielectric relaxor behavior and improves the piezoelectric properties simultaneously. The 0.2PZN–0.8PZT with 0.5 wt% NiO addition shows good transduction coefficient (d₃₃·g₃₃ = 10,050 × 10^?15 m²/N) and large fracture toughness (K_IC = 1.35 MPa m^1/2).     

Improvement of the hydroxyapatite mechanical properties by direct microwave sintering in single mode cavity

The main purpose of this study consists in investigating the direct microwave sintering of hydroxyapatite (HA) in a single mode cavity. Firstly, stoichiometric HA powders were synthesized by a coprecipitation method from diammonium phosphate and calcium nitrate solutions and shaped by slip-casting. Then, using the one-step microwave process, dense pellets with fine microstructures were successfully obtained in short sintering timespan. A parametric study permitted to determine the influence of powder grain size, sintering temperature and dwell time on the sintered samples microstructures. The Young's modulus (E) and hardness (H) were measured by nanoindentation and the values discussed according to the microstructure. Finally, the resulting mechanical properties determined on the microwave sintered samples (E = 148.5 GPa, H = 9.6 GPa, σ_compression = 531.3 MPa and K_IC = 1.12 MPa m^1/2) are significantly higher than those usually reported in the literature, whatever the sintering process, and could allow the use of HA for structural applications.     

Novel low-κ polyimide/mesoporous silica composite films: Preparation,microstructure, and properties

A series of novel low-dielectric constant (low-κ) polyimide (PI) composite films containing the SBA-15 or the SBA-16-type mesoporous silica were successfully prepared via in situ polymerization and following thermal imidization. Their morphologies, dielectric constants, and thermal and dynamic mechanical properties were investigated. It is found that the dielectric constants of the composite films can be reduced from 3.34 of the pure PI to 2.73 and 2.61 by incorporating 3 wt% SBA-15 and 7 wt% SBA-16, respectively. The reduction of the dielectric constant is attributed to the incorporation of the air voids (κ = 1) stored within the mesoporous silica materials, the air volume existing in the gaps on the interfaces between the mesoporous silica and the PI matrix, and the free volume created by introducing large-sized domains. The PI/mesoporous silica composite films prepared in this study also present stable dielectric constants across the wide frequency range and a good phase interconnection. The improvement of the thermal stability and dynamic mechanical properties of the PI film is achieved by incorporation of the mesoporous silica materials. The enhanced interfacial interaction between the surface-treated mesoporous silica and the PI matrix has led to the minimization of the deterioration of the mechanical properties. The incorporation of the mesoporous silica materials is a promising approach to prepare the low-κ PI films.     

Role of cement content on the properties of self-flowing Al2O3 refractory castables

In this work, Al₂O₃ self-flowing castables (SFCs) were produced based on various cement contents. The SFCs were sintered at 1273 K, 1573 K and 1773 K and the exhibited properties were experimentally determined. Among the properties determined in this work are bulk density (BD), apparent porosity (AP), water absorption (WA), cold crushing strength (CCS), modulus of rupture (MOR) and fracture toughness (K_IC). It is found that additions of 5% cement lead to SFCs with maximum MOR and K_IC values after firing at 1773 K. Firing at 1573 K leads to a reduction in both, MOR and K_IC. In SFC containing 3% cement, maximum K_IC values of 3.53 MPa m^1/2 were achieved after firing at 1573 K. In the low cement SFCs (1 wt%) after firing at 1773 K the exhibited K_IC values were below those obtained in either the SFC-3 or SFC-5, but they were significantly high (3.43 MPa m^1/2).     

Enhanced thermoelectric properties of CNT dispersed and Na-doped Bi2Ba2Co2Oy composites

The thermoelectric properties of Bi₂Ba₂Co₂O_y and Bi_1.975Na_0.025Ba₂Co₂O_y+x wt% carbon nanotubes (CNT; x=0.00, 0.05, 0.10, 0.15, 0.5, and 1.0) ceramic samples synthesised by the solid-state reaction method were investigated from 300K to 950K. Na doping with a small amount played an important role in reducing resistivity and slightly reduced the Seebeck coefficients and the thermal conductivity. The CNT dispersant increased resistivity, but the thermal conductivity was reduced remarkably. In particular, the Bi_1.975Na_0.025Ba₂Co₂O_y+1.0wt% CNT sample exhibited an ultralow thermal conductivity of 0.39 W K⁻¹ m⁻¹ at 923K. This was attributed to the point defects caused by Na doping and the interface scattering caused by the CNT dispersant. The combination of Na doping and CNT dispersion had better effects on thermoelectric properties. The Bi_1.975Na_0.025Ba₂Co₂O_y+0.5wt% CNT sample exhibited a better dimensionless figure of merit (ZT) value of 0.2 at 923K, which was improved by 78.2%, compared with the undoped Bi₂Ba₂Co₂O_y sample.     

Tailoring carbon nanotube/matrix interface to optimize mechanical properties of multiscale composites

Pyrolytic carbon (PyC) was deposited on surfaces of carbon nanotubes (CNT) which were grown on carbon fibers to optimize the interfacial bonding between CNT/Matrix. The PyC protected CNT effectively and weakened CNT/Matrix interfacial strength, leading to long pull-out of CNT compared to brittle fracture of uncoated CNT. The well-protected CNT have more effective contributions to the improvement of mechanical properties. A “fiber-PyC/SiC-(CNT + PyC)-(CNT + SiC)” structure was formed using this process.     

Influence of experimental variables on fracture toughness determined on SEVNB in three points bending. Mullite a case study

The effect of testing variables on toughness of single edge “V” notched beams (4 mm × 6 mm × 50 mm, α = 0.6) of a fine grained mullite (d₅₀ = 0.7 ± 0.5 μm) in three points bending (span = 40 mm) is analysed. Mullite was selected as case material because it presents flat R-curve and subcritical crack propagation. Stable fracture was reached by using the CMOD as control variable (0.001 and 0.018 mm/min). Results for stable test and unstable displacement (0.05 mm/min) controlled tests are analysed. K_IC has been calculated from maximum loads, K_ICp, and from the total fracture energy determined in stable tests, K_ICγ. The fact that for materials with flat R-curve both K_IC values are coincident has been used as criterion for adequacy of the test. Stable fracture at high deformation rates is required to fulfil K_ICp = K_ICγ. Under such conditions, an intrinsic K_IC = 0.86 ± 0.06 MPa m^1/2, less than one half of those previously reported has been obtained.     

On the manufacturing and electrical and mechanical properties of ultra-high wt.% fraction aligned MWCNT and randomly oriented CNT epoxy composites

The effect of CNT orientation on electrical and mechanical properties is presented on the example of an ultra-high filler loaded multi-walled carbon nanotube (68 wt.% MWCNTs) epoxy-based nanocomposite. A novel manufacturing method based on hot-press infiltration through a semi-permeable membrane allows to obtain both, nanocomposites with aligned and randomly oriented CNTs (APNCs and RPNCs) over a broad filler loading range of ≈10–68 wt.%. APNCs are based on low-defected, mm-long aligned MWCNT arrays grown in chemical vapour deposition (CVD) process. Electrical conductivity and mechanical properties were measured parallel and perpendicular to the direction of CNTs. RPNCs are based on both, aligned mm-long MWCNTs and randomly oriented commercial μm-long and entangled MWCNTs (Baytube C150P, and exemplarily Arkema Graphistrength C100). The piezoresistive strain sensing capability of these high-wt.% APNCs and RPNCs had been investigated towards the influence of CNT orientations. For the highest CNT fraction of 68 wt.% of unidirectional aligned CNTs a Young’s modulus of E_|| ≈ 36 GPa and maximum electrical conductivity of σ_|| ≈ 37·10⁴ S/m were achieved.     

Fabrication and mechanical properties of short ZrO2 fiber reinforced NiFe2O4 matrix composites

Short ZrO₂ fibers (ZrO_2(f)) reinforced NiFe₂O₄ ceramic composites were fabricated by cold pressing process. The phase composition, microstructure, mechanical properties and fiber/matrix interface of the composites were investigated by X-ray diffraction, scanning electron microscopy and mechanical testing machines. ZrO_2(f) show good thermodynamic and chemical compatibility with NiFe₂O₄ ceramic matrix and effectively enhanced the mechanical properties. The toughening mechanisms are fiber bridging, interfacial debonding, fiber pullout, phase transformation and the matrix constraint effect. By incorporation of 3 wt% fibers with the average length of 5～6 mm, the bending strength and fracture toughness of the composites reached 88.92 MPa and 4.62 MPa m^1/2, respectively, while the strength conservation ratio after thermal shock increased from 48.85% to 75.86%. The weak interface bonding built up between ZrO_2(f) and NiFe₂O₄ facilitates the reinforcing effects of the fibers to operate.     

Room and high temperature flexural failure of spark plasma sintered boron carbide

Dense (95–98.6%) bulk boron carbide prepared by Spark Plasma Sintering (SPS) in Ar or N₂ atmospheres were subject to three-point flexural tests at room and at 1600 °C. Eight different consolidation conditions were used via SPS of commercially available B₄C powder. Resulting specimens had similar grain size not exceeding 4 µm and room-temperature bending strength (σ_25 °C) of 300–600 MPa, suggesting that difference in σ_25 °C is due to development of secondary phases in monolithic boron carbide ceramics during SPS processing. To explain such difference the composition of boron carbide and secondary phases observed by XRD and Raman spectroscopy. The variation in intensity of the Raman peak at 490 cm⁻¹ of boron carbide suggests modification of the boron carbide composition and a higher intensity correlates with a higher room-temperature bending strength (σ_25 °C) and Vickers hardness (HV). Secondary phases can modify the level of mechanical characteristics within some general trends that are not dependent on additives (with some exceptions) or technologies. Namely, HV increases, σ_25 °C decreases, and the ratio σ_1600 °C/σ_25 °C (σ_1600 °C – bending strength at 1600 °C) is lower when fracture toughness (K_IC) is higher. The ratio σ_1600 °C/σ_25 °C shows two regions of low and high K_IC delimited by K_IC=4.1 MPa m^0.5: in the low K_IC region, boron carbide specimens are produced in nitrogen.     

Improved mechanical performance of solution-processed MWCNT/Ag nanoparticle composite films with oxygen-pressure-controlled annealing

A method for the synthesis of solution process-based MWCNT/Ag nanoparticle composite thin films as electrode or interconnect materials for flexible electronic devices is presented. The method produces homogeneously-dispersed CNT networks and increases the density of the Ag matrix, which are major factors in determining the mechanical performance of CNT/Ag films. By introducing nanometer-sized Ag particles as a matrix material, the agglomeration of CNTs is suppressed. In addition, the generation of pores during the synthesis procedure is effectively restrained by oxygen-pressure-controlled annealing. The elastic modulus of the pristine Ag films was observed to increase by 34% by adding 5 wt% CNTs. An improvement in the fatigue resistance of the CNTs under cyclic tensile deformation was confirmed. The normalized resistance change ((R ? R_o)/R_o) of the Ag films containing 5 wt% CNTs after fatigue testing was reduced by about 27% compared to that of the pristine Ag films. For industrial application the process has the advantage of relatively low-temperature processing without any high pressure compaction compared to the conventional powder metallurgy techniques normally used.     

Polyethylene/octa-(ethyl octadeca-10,13 dienoamide) silsesquioxane blends and the adhesion strength to paperboard

Octa-(ethyl octadeca-10,13 dienoamide) silsesquioxane or bio-POSS was used in the fabrication of polyethylene (PE)/bio-POSS blends by melt mixing. These PE/bio-POSS blends were applied to paperboard by compression moulding coating. The T-peel test was used to determine the adhesion of the blends to paperboard. A FTIR-ATR spectroscopic study was performed to identify the interfacial interaction between PE/bio-POSS blends and paperboard. The T-peel test showed that the adhesion of PE to paperboard was enhanced when there was less than 10 wt% of bio-POSS in the blends. The best adhesions were achieved at 5 wt% and 3 wt% bio-POSS, coated at 200 °C/20 °C and 300 °C/20 °C, respectively. The increase in adhesion strength was attributed to the contribution of mechanical interlocks and probable interfacial interaction between amide groups of bio-POSS and hydroxyl groups of paperboard, as specified by FTIR-ATR. Bio-POSS content above 10 wt% led to a decrease in adhesion between PE/bio-POSS blends and paperboard because the melt flows and mechanical properties of the blends were dramatically decreased.     

Carbon nanotube toughened aluminium oxide nanocomposite

This paper describes the mechanical properties of carbon nanotube-reinforced Al₂O₃ nanocomposites fabricated by hot-pressing. The results showed that compared with monolithic Al₂O₃ the fracture toughness, hardness and flexural strength of the nanocomposites were improved by 94%, 13% and 6.4% respectively, at 4 vol.% CNT additions. For 10 vol.% CNT additions, with the exception of the fracture toughness, which was improved by 66%, a decrease in mechanical properties was observed when compared with those for monolithic Al₂O₃. The toughening mechanism is discussed, which is due to the uniform dispersion of CNTs within the matrix, adequate densification, and proper CNT/matrix interfacial connections.     

EELS characterisation of β-tricalcium phosphate and hydroxyapatite

Hydroxyapatite (HA) and β-tricalcium phosphate (β-TCP) are of great interest due to their potential application as bone-replacement materials. In particular, composites made of a mixture of these Ca-phosphates revealed improved mechanical properties; however, the reason for this improvement is unknown. Future development and properties enhancement of such bioceramics is linked to the possibility to characterise their particular microstructure. In this context, the ability to quickly identify individual grains of HA and β-TCP within these composites will allow acquiring information about the phase distributions and the phase-boundary microstructure. The aim of the present study is, therefore, to demonstrate that electron energy-loss spectroscopy (EELS) can be successfully employed to differentiate between individual grains of HA and β-TCP. In particular, the analysis of the near-edge structure of the oxygen K-ionisation edge allows detection of a characteristic signal at ca. 536 eV that can be employed as an identification tool for HA. EELS investigations were performed first on as-received and calcined (1000 °C) HA and β-TCP powders and subsequently on pure bulk HA and β-TCP samples sintered at 1250 °C. Finally, this method was successfully applied to a HA/β-TCP (50/50 wt.%) composite sintered at 1250 °C.