Thermomechanical properties of bio-based composites made from a lactic acid thermoset resin and flax and flax/basalt fibre reinforcements

Low viscosity thermoset bio-based resin was synthesised from lactic acid, allyl alcohol and pentaerythritol. The resin was impregnated into cellulosic fibre reinforcement from flax and basalt and then compression moulded at elevated temperature to produce thermoset composites. The mechanical properties of composites were characterised by flexural, tensile and Charpy impact testing whereas the thermal properties were analysed by dynamic mechanical thermal analysis (DMTA) and thermogravimetric analysis (TGA). The results showed a decrease in mechanical properties with increase in fibre load after 40 wt.% for the neat flax composite due to insufficient fibre wetting and an increase in mechanical properties with increase fibre load up to 60 wt.% for the flax/basalt composite. The results of the ageing test showed that the mechanical properties of the composites deteriorate with ageing; however, the flax/basalt composite had better mechanical properties after ageing than the flax composite before ageing.     

Retention of mechanical performance of polymer matrix composites above the glass transition temperature by vascular cooling

An actively cooled vascular polymer matrix composite containing 3.0% channel volume fraction retains greater than 90% flexural stiffness when exposed continuously to 325 °C environmental temperature. Non-cooled controls suffered complete structural failure through thermal degradation under the same conditions. Glass–epoxy composites (T_g = 152 °C) manufactured by vacuum assisted resin transfer molding contain microchannel networks of two different architectures optimized for thermal and mechanical performance. Microchannels are fabricated by vaporization of poly(lactide) fibers treated with tin(II) oxalate catalyst that are incorporated into the fiber preform prior to resin infiltration. Flexural modulus, material temperature, and heat removal rates are measured during four-point bending testing as a function of environmental temperature and coolant flow rate. Simulations validate experimental measurements and provide insight into the thermal behavior. Vascular specimens with only 1.5% channel volume fraction centered at the neutral bending axis also retained over 80% flexural stiffness at 325 °C environmental temperature.     

Assessment of three oxide/oxide ceramic matrix composites: Mechanical performance and effects of heat treatments

Mechanical performance of three oxide/oxide ceramic matrix composites (CMCs) based on Nextel 610 fibers and SiOC, alumina, and mullite/SiOC matrices respectively, is evaluated herein. Tensile strength and stiffness of all materials decreased at 1000 °C and 1200 °C, probably because of degradation of fiber properties beyond 1000 °C. Microstructural changes in the composites during exposure at 1000 °C and 1200 °C for 50 h reduce their flexural strength, fracture toughness and work of fracture. A literature review regarding mechanical properties of several oxide/oxide CMCs revealed lower influence of fiber properties on composite strength compared with elastic modulus. The tested composites exhibit comparable stiffness and strength but higher fracture toughness compared with average values determined from a literature review. Considering CMCs with different compositions, we observed an interesting linear trend between strength and fracture toughness. The validity of the linear relationship between fracture strength and flexural toughness for CMCs is discussed.     

Ductile unidirectional continuous rayon fibre-reinforced hierarchical composites

Endless rayon fibres (Cordenka®) were used to reinforce polyhydroxybutyrate (PHB) nanocomposites containing 2.5 wt.% nanofibrillated cellulose (NFC) to create truly green hierarchical composites. Unidirectional (UD) composites with 50–55% fibre volume fraction were produced using a solvent-free continuous wet powder impregnation method. The composites exhibit ductile failure behaviour with a strain-to-failure of more than 10% albeit using a very brittle matrix. Improvements at a model composite level were translated into higher mechanical properties of UD hierarchical composites. The Young’s moduli of rayon fibre-reinforced (NFC-reinforced) PHB composites were about 15 GPa. The tensile and flexural strength of hierarchical PHB composites increased by 15% and 33% as compared to the rayon fibre-reinforced neat PHB composites. This suggests that incorporation of NFC into the PHB matrix binds the rayon fibres, which does affect the load transfer between the constituents resulting in composites with better mechanical properties.     

Soybean oil-based thermosets with N-vinyl-2-pyrrolidone as crosslinking agent for hemp fiber composites

Soybean oil-based thermosets from acrylated epoxidized soybean oil (AESO) with a highly reactive vinyl monomer, N-vinyl-2-pyrrolidone (NVP), as crosslinking agent to replace styrene (St) were formulated for the fabrication of hemp fiber composites. The theoretical miscibility of NVP–AESO and St–AESO systems were discussed based on the group contribution method. The AESO resin with 30 wt% NVP exhibited a slightly higher viscosity than the counterpart with St, while the maximum curing temperature of the former was considerably lower than that of the latter. The composites from 20 wt% NVP resin gained comparable mechanical properties and higher glass transition temperature (T_g) to the composites with 30 wt% St. Further increase in NVP usage to 40 wt% resulted in the composites with higher tensile strength, tensile modulus, flexural strength, flexural modulus, storage modulus, and T_g of 29.6%, 22.4%, 22.5%, 20.6%, 21.6%, and 47.2%, respectively, when compared to those of the St-based composites.     

Survival of actively cooled microvascular polymer matrix composites under sustained thermomechanical loading

Exposure to high heat can cause polymer matrix composites (PMC) to fail under mechanical loads easily sustained at room temperature. However, heat is removed and temperature reduced in PMCs by active cooling through an internal vascular network. Here we compare structural survival of PMCs under thermomechanical loading with and without active cooling. Microchannels are incorporated into autoclave-cured carbon fiber/epoxy composites using sacrificial fibers. Time-to-failure, material temperature, and heat removal rates are measured during simultaneous heating on one face (5–75 kW/m²) and compressive loading (100–250 MPa). The effects of applied compressive load, heat flux, channel spacing, coolant flow rate, and channel distance from the heated surface are examined. Actively cooled composites containing 0.33% channel volume fraction survive without structural failure for longer than 30 min under 200 MPa compressive loading and 60 kW/m² heat flux. In dramatic comparison, non-cooled composites fail in less than a minute under the same loading conditions.     

Hybridization effect on the mechanical properties of curaua/glass fiber composites

The aim of this paper was to evaluate the effect of hybridizing glass and curaua fibers on the mechanical properties of their composites. These composites were produced by hot compression molding, with distinct overall fiber volume fraction, being either pure curaua fiber, pure glass fiber or hybrid. The mechanical characterization was performed by tensile, flexural, short beam, Iosipescu and also nondestructive testing. From the obtained results, it was observed that the tensile strength and modulus increased with glass fiber incorporation and for higher overall fiber volume fraction (%V_f). The short beam strength increased up to %V_f of 30 vol.%, evidencing a maximum in terms of overall fiber/matrix interface and composite quality. Hybridization has been successfully applied to vegetable/synthetic fiber reinforced polyester composites in a way that the various properties responded satisfactorily to the incorporation of a third component.     

Environmental resistance of flax/bio-based epoxy and flax/polyurethane composites manufactured by resin transfer moulding

As biocomposites are highly sensitive to water absorption, the aim of this study was to compare the physical properties two biocomposites: (1) a flax/bio-based epoxy (Entropy SUPER SAP CLR/INS) and (2) a flax/polyurethane (HENKEL LOCTITE MAX 3). Both materials were reinforced with 14 layers of flax (TEXONIC twill 2 × 2) and manufactured using a resin transfer moulding process. Post-cured composite samples were aged at 90% RH and 30 °C for various periods of time up to 720 h. The results showed that both composites followed a Fickian diffusion behaviour. Water had a plasticizing effect on the composites and it changed their failure mode. This effect took longer to appear for the polyurethane composites. The chemical bonds between the hydroxyl groups of the fibres and the isocyanate lead to a stronger interface which improved the mechanical properties (short beam and compressive strengths) as compared to the flax/bio-epoxy composites.     

Grafting of nano-TiO2 onto flax fibers and the enhancement of the mechanical properties of the flax fiber and flax fiber/epoxy composite

In this article, a flax fiber yarn was grafted with nanometer sized TiO₂, and the effects on the tensile and bonding properties of the single fibers and unidirectional fiber reinforced epoxy plates were studied. The flax fiber yarn was grafted with nanometer sized TiO₂ through immersion in nano-TiO₂/KH560 suspensions under sonification. The measured grafting content of the nano-TiO₂ ranged from 0.89 wt.% to 7.14 wt.%, dependent on the suspension concentration. With the optimized nano-TiO₂ grafting content (∼2.34 wt.%), the tensile strength of the flax fibers and the interfacial shear strength to an epoxy resin were enhanced by 23.1% and 40.5%, respectively. The formation of Si–O–Ti and C–O–Si bonds and the presence of the nano-TiO₂ particles on the fiber surfaces contributed to the property enhancements. Unidirectional flax fiber reinforced epoxy composite (V_f = 35.4%) plates prepared manually showed significantly enhanced flexural properties with the grafting of nano-TiO₂.     

The effect of reprocessing on the mechanical properties of polypropylene reinforced with wood pulp,flax or glass fibre

Composites of polypropylene, substitutable for a given application and reinforced with: Medium Density Fibreboard fibre (MDF) (40 wt%); flax (30 wt%); and glass fibre (20 wt%), were evaluated after 6 injection moulding and extrusion reprocessing cycles. Of the range of tensile, flexural and impact properties examined, MDF composites showed the best mean property retention after reprocessing (87%) compared to flax (72%) and glass (59%). After 1 reprocessing cycle the glass composite had higher tensile strength (56.2 MPa) compared to the MDF composite (44.4) but after 6 cycles the MDF was stronger (35.0 compared to 29.6 MPa for the glass composite). Property reductions were attributed to reduced fibre length. MDF fibres showed the lowest reduction in fibre length between 1 and 6 cycles (39%), compared to glass (51%) and flax (62%). Flax fibres showed greater increases in damage (cell wall dislocations) with reprocessing than was shown by MDF fibres.     

Greatly enhanced cryogenic mechanical properties of short carbon fiber/polyethersulfone composites by graphene oxide coating

In order to employ polyethersulfone (PES) in cryogenic engineering field, its cryogenic mechanical performance should be examined and should also be improved to meet the high requirement for cryogenic engineering application. In this work, pure PES, graphene oxide (GO)/PES, short carbon fiber (SCF)/PES, GO/SCF/PES and GO-coated SCF/PES composites are prepared using the extrusion compounding and injection molding techniques. The tensile and flexural properties of these composites are systematically investigated at a typical cryogenic temperature (77 K). It is shown that the cryogenic mechanical properties are enhanced by the addition of GO, SCFs and coated-SCFs. In particular, the GO-coated SCF/PES composites display the greatly enhanced cryogenic mechanical properties with the highest values compared to other PES composites. In addition, it is exhibited that the cryogenic mechanical properties at 77 K of PES and its composites are far higher than those at room temperature (RT).     

Fabrication and characterization of 3-D Cf/ZrC composites by low-temperature liquid metal infiltration

Three-dimensional braided carbon fiber-reinforced ZrC matrix composite, 3-D C_f/ZrC, were prepared by liquid metal infiltration process at 1200 °C using a Zr₂Cu intermetallic compound as infiltrator. The microstructure and properties of the composites were investigated. The results indicated that ZrC with a yield of 35.2 ± 1.8 vol.% was certified as the major phase of the composites. The formation of ZrC was controlled by a solution-precipitation mechanism. The obtained composites exhibited good mechanical properties, with a flexural strength of 293.0 ± 12.1 MPa, a flexural modulus of 82.7 ± 6.4 GPa and a fracture toughness of 9.8 ± 0.9 MPa m^1/2. The mass and linear ablation rates of the composites exposed to oxyacetylene torch were 0.0013 ± 0.0005 g s⁻¹ and −0.0009 ± 0.0003 mm s⁻¹, respectively. The formation of a dense ZrO₂ protective layer and the evaporation of residual Cu contributed mainly to the excellent ablation resistance.     

Structural and thermal characterization of Moroccan sugar cane bagasse cellulose fibers and their applications as a reinforcing agent in low density polyethylene

Cellulose fibers were isolated from Moroccan sugar cane bagasse by using three distinct stages. Firstly bagasse was subjected to (1) a hot water (70 °C) treatment to eliminate hemicellulose, then to (2) an alkaline aqueous solution (15% of sodium hydroxide (NaOH), 98 °C) treatment to eliminate lignin, and finally to (3) a bleaching stage. Sugar cane bagasse cellulose fibers were analyzed by different complementary analysis (FT-IR; ¹³C NMR and TG). The reinforcing capability of cellulose fibers extracted from sugar cane bagasse was investigated using low density polyethylene as matrix. The cellulosic preparations were free of bound lignin. The intrinsic viscosity, the viscosity average and the molecular weight were respectively 511 ml/g, 1769 and 286578 g/mol. An enhance on mechanical properties of composites was found, a gain of 72% in Young’s modulus at 25 wt.% fiber loading and a gain of 85% in flexural modulus at 25 wt.% fiber loading, as a results of a good interface adhesion between cellulose fibers and matrix.     

Size-scale effects of silica on bis-GMA/TEGDMA based nanohybrid dental restorative composites

The present study focuses on the effect of size-scale combination of silica on the mechanical and dynamic mechanical properties of acrylate based (50% Bis-GMA and 50% TEGDMA by weight) composites with an aim to overcome the conventional problem of high-volume fraction filling of acrylate based composites, typically used in restorative dentistry. Two classes of light-cured composites based on the size-scale combination of silica (7 nm + 2 μm; 14 nm + 2 μm) as the filler were prepared. FTIR spectroscopy revealed functionality and interactions whereas morphological investigations concerning the state of distribution and dispersion of nano- and micro-silica has been carried out by SEM–EDX Si-dot mapping. The dynamic mechanical properties, compressive, flexural and diametral tensile strengths were characterized. Micromechanical analysis of viscoelastic storage moduli following Kerner composite model has revealed an enhancement in the reinforcement efficiency of the nanohybrid composites based on the filler size-scale combination of 14 nm + 2 μm with 10 wt.% nanofiller loading. The compressive strength of the micro-filled composite (with 2 μm silica only) was found to remain comparable to that of the nanohybrid with 5 wt.% of 7 nm silica and 10 wt.% of 14 nm silica filled composites. Diametral tensile strength has been observed to be influenced by the size-scale combination and extent of nanofiller loading. The effective volume fractions in the composites validating the experimentally determined DTS were calculated following Nicolais–Narkis model. Our study demonstrates the conceptual feasibility of exploring the optimization of size-scale combinations of filler for enhancement in reinforcement efficiency by manipulating the volume fraction of filler induced immobilized polymer chains by resorting to the principle of micromechanics.     

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

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

Microstructure and mechanical properties of an Al–TiC metal matrix composite obtained by reactive synthesis

A metal matrix composite has been obtained by a novel synthesis route, reacting Al₃Ti and graphite at 1000 °C for about 1 min after ball-milling and compaction. The resulting composite is made of an aluminium matrix reinforced by nanometer sized TiC particles (average diameter 70 nm). The average TiC/Al ratio is 34.6 wt.% (22.3 vol.%). The microstructure consists of an intimate mixture of two domains, an unreinforced domain made of the Al solid solution with a low TiC reinforcement content, and a reinforced domain. This composite exhibits uncommon mechanical properties with regard to previous micrometer sized Al–TiC composites and to its high reinforcement volume fraction, with a Young’s modulus of ∼110 GPa, an ultimate tensile strength of about 500 MPa and a maximum elongation of 6%.     

Effects of high-temperature annealing on the microstructure and properties of C/SiC–ZrB2 composites

C/SiC–ZrB₂ composites prepared via precursor infiltration and pyrolysis (PIP) were treated at high temperatures ranging from 1200 °C to 1800 °C. The mass loss rate of the composites increased with increasing annealing temperature and the flexural properties of the composites increased initially and then decreased reversely. Out of the four samples, the flexural strength and the modulus of the specimen treated at 1400 °C are maximal at 216.9 MPa and 35.5 GPa, suggesting the optimal annealing temperature for mechanical properties is 1400 °C. The fiber microstructure evolution during high-temperature annealing would not cause the decrease of fiber strength, and moderate annealing temperature enhanced the thermal stress whereas weakened the interface bonding, thus boosting the mechanical properties. However, once the annealing temperature exceeded 1600 °C, element diffusion and carbothermal reduction between ZrO₂ impurity and carbon fibers led to fiber erosion and a strong interface, jeopardizing the mechanical properties of the composites. The mass loss rate and linear recession rate of composites treated at 1800 °C are merely 0.0141 g/s and 0.0161 mm/s, respectively.     

The optimal formulation of recycled polypropylene/rubberwood flour composites from experiments with mixture design

A mixture design was used in experiments, to determine the optimal mixture for composites of rubberwood flour (RWF) and reinforced recycled polypropylene (rPP). The mixed materials were extruded into panels. Effects were determined of the mixture components rPP, RWF, maleic anhydride-grafted polypropylene (MAPP), and ultraviolet (UV) stabilizer, on the mechanical properties. The overall composition significantly affected flexural, compressive, and tensile properties. The fractions of recycled polypropylene and rubberwood flour increased all the mechanical material properties; however, increasing one fraction must be balanced by decreasing the other, and the rubberwood flour fraction had a higher effect size. The fraction of MAPP was best kept in mid-range of the fractions tested, while the UV stabilizer fraction overall degraded the mechanical properties. Our results suggest that the fraction of UV stabilizer should be as small as possible to minimize its negative influences. The models fitted were used for optimization of a desirability score, substituting for the multiple objectives modeled. The optimal formulation found was 50.3 wt% rPP, 44.5 wt% RWF, 3.9 wt% MAPP, 0.2 wt% UV stabilizer, and 1.0 wt% lubricant; the composite made with this formulation had good mechanical properties that closely matched the model predictions.     

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

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

Novel method for determination of critical fiber length in short fiber carbon/carbon composites by double lap joint

A novel approach is introduced for the experimental determination of critical fiber length in carbon fiber reinforced carbon (CFRC) composites. Critical fiber length is investigated using double lap joint samples. The transition of failure mode from bonding failure to fiber fraction with increasing overlap length correlates with the critical fiber length. Tested overlap lengths were in the range of 4–100 mm. For CFRC at hand, failure mode changes at an overlap length of 26 ± 2 mm. Hence critical fiber length is derived as l_c = 52 ± 4 mm.