Mechanical Behaviour of As-Manufactured and Repaired Aligned Discontinuous Basalt Fibre-Reinforced Vitrimer Composites.

The aim of this research is to investigate basalt as a natural mineral-based fibre together with a vitrimeric resin as a sustainable alternative to standard composite materials. Vitrimers combine the properties of thermoset and thermoplastic polymers, enabling the repair of specimens and hence prolonging the lifetime of the composite material. The micro-mechanical characteristics between the basalt fibres and the vitrimer resin are reported and shown to match those of a standard Skyflex K51 epoxy resin. Discontinuous (4 mm) basalt fibres were employed to produce aligned discontinuous fibre-reinforced composites (ADFRCs) using the high-performance discontinuous fibre (HiPerDiF) technology. The mechanical characteristics of the laminates were investigated through tensile testing and the fracture zones were analysed under a scanning electron microscope. By normalising the results by their respective fibre volume fraction, it was discovered that the vitrimer-basalt ADFRCs exhibited, on average, a 4% higher strength and a 25% higher stiffness compared to their basalt epoxy counterparts. The repair potential of the vitrimer ADFRC specimens was explored during low-temperature compression repair. Two approaches were tested using double-sided local- and full-patch repair. Both successfully recovered a significant amount of their prime strength. In conclusion, the potential of the sustainable vitrimer-basalt composite is shown by its competitive mechanical performance. Combining this with the manufacturing flexibility, repair potential, and recyclability of the material, the vitrimer-basalt composite seems to be a competitive alternative to standard glass epoxies.

Influence of the Second-Phase Resin Structure on the Interfacial Shear Strength of Carbon Fiber/Epoxy Resin.

The toughening modification of epoxy resin has received widespread attention. The addition of the second-phase resin has a good toughening effect on epoxy resin. In order to investigate the effect of the second-phase resin on the interphase of composites, in this work the interfacial properties of carbon fiber (CF)/epoxy resin with the second-phase resin structure were investigated. Methodologies including surface structure observation, chemical characteristics, surface energy of the CF, and micro-phase structure characterization of resin were tested, followed by the micro-interfacial performance of CF/epoxy composites before and after hygrothermal treatment. The results revealed that the sizing process has the positive effect of increasing the interfacial bonding properties of CF/epoxy. From the interfacial shear strength (IFSS) test, the introduction of the second phase in the resin reduced the interfacial bonding performance between the CF and epoxy. After the hygrothermal treatment, water molecules diffused along the interfacial paths between the two resins, which in turn created defects and consequently brought about a reduction in the IFSS.

Improving the Accuracy of the Evaluation Method for the Interfacial Shear Strength of Fiber-Reinforced Thermoplastic Polymers through the Short Beam Shear Test.

Short fiber-reinforced thermoplastic polymers (SFRTPs) are commonly used in various molding methods due to their high specific elasticity and strength. To evaluate the interfacial strength, several determination methods have been proposed, including the interfacial shear strength (IFSS). In previous research, an IFSS evaluation method based on the short beam shear method was proposed. However, this method is only applicable to micrometer-sized fibers with high stiffness levels that are not easily bent. When utilizing cellulose fiber, the interfacial shear strength (IFSS) results frequently exhibit significant deviations. To tackle this issue, we suggest an enhanced experimental technique that employs beam-shaped specimens with welding points based on the short beam shear test. Furthermore, we conducted a three-dimensional analysis of the original method to determine the fiber orientation angle and IFSS. The outcomes were compared with previously reported determinations. The IFSS achieved through the novel method proposed in this paper exhibits high precision and reliability, rendering it suitable for use with soft and flexible fibers.

Improvement and Evaluation of a Device That Determines the Interfacial Shear Strength of Carbon Fiber/Polyphenylene Sulfide Composites.

This study improved homemade apparatus for characterizing the interfacial shear strength (IFSS) of carbon-fiber-reinforced polyphenylene sulfide (PPS/CF) composites. The upgraded generation II experimental device includes a newly developed experimental clamp for samples, as well as testing systems. Compared with the initial generation I apparatus and the commercial Toei instrument, the generation II device is easier and more efficient to operate. The average interfacial adhesion values obtained using these devices were consistently approximately 40 MPa, with relatively low data scatter, showing excellent repeatability and applicability during microbond tests. Notably, the generation II experimental device was equipped with an additional high-frequency data-capturing tool to identify the debonding peak force more precisely, which demonstrated a higher interfacial shear strength of 42.81 MPa during testing. Therefore, the new instrument was able to reflect the change in the interfacial stress state during the interface debonding process more accurately and reliably.

Enhanced Interfacial Properties of Carbon Fiber/Maleic Anhydride-Grafted Polypropylene Composites via Two-Step Surface Treatment: Electrochemical Oxidation and Silane Treatment.

The interfacial adhesion between carbon fibers (CFs) and a thermoplastic matrix is an important aspect that should be improved in manufacturing CF-reinforced thermoplastics with high strength and rigidity. In this study, the effects of a two-step surface treatment comprising electrochemical oxidation and silane treatment of the CF surface on the mechanical properties of CF/maleic anhydride-grafted polypropylene (MAPP) composites were confirmed. The surface characteristics of the treated CFs were analyzed via scanning electron microscopy, atomic force microscopy, Fourier transform infrared spectroscopy, and X-ray photoelectron spectroscopy. The tensile testing of a single CF and interfacial adhesion of the samples before and after the surface treatment were analyzed using a single-fiber testing machine and a universal testing machine. After the silane treatment, the roughness of the CF surface increased due to the formation of a siloxane network. In addition, the interfacial shear strength increased by ∼450% compared to that of the untreated CFs due to the covalent bond between the -NH2 end group of siloxane and MAPP. This two-step surface treatment, which can be performed continuously, is considered an effective method for improving the mechanical interface strength between the CF and polymer matrix.

Impact Energy Dissipation and Quantitative Models of Injection Molded Short Fiber-Reinforced Thermoplastics.

Glass short fiber-reinforced thermoplastics (SGFRTP) are used to reduce carbon dioxide emissions from transportation equipment, especially household vehicles. The mechanical properties required for SGFRTP include flexural strength, impact resistance, etc. In particular, impact resistance is an important indicator of the use of SGFRTP. For this study, a mechanical model was developed to explain the notched impact strength of SGFRTP injection molded products in terms of their interfacial shear strength. The values obtained from the model show good agreement with the experimentally obtained results (R2 > 0.95). Results also suggest that the model applies to different fiber orientation angle and a range of fiber lengths in the molded product that are sufficiently shorter than the critical fiber length.

Preparation and Interfacial Properties of Hydroxyl-Containing Polyimide Fibers.

Developing polyimide (PI) fibers with excellent interfacial adhesion and high mechanical properties for the PI fiber-reinforced polymer matrix composites (PFRPs) industry has been challenging. In this work, 4,4'-diamino-(1,1'-biphenyl)-3,3'-diol (HAB) diamine was introduced into the rigid molecular chains, and the high-performance PI fibers, presenting an interfacial shear strength (IFSS) value of 46.33 MPa, tensile strength of 2.62 GPa, and modulus of 100.15 GPa, were successfully manufactured when the content of HAB in mixed diamines was 30 mol %. Fourier transform infrared (FTIR) spectroscopy identified the presence of intermolecular H-bonding interactions, and 2D small-angle X-ray scattering indicated that the introduction of HAB moiety contributed to reducing the radii of microvoids in the fibers, which were considered to be the key factors leading to a significant enhancement in the mechanical properties of the fibers. X-ray photoelectron spectroscopy (XPS) and the static contact angle intuitively illustrated that the synthetic fiber surface contained active hydroxyl groups. The IFSS value of PI fiber/epoxy resin composites (PI/EPs) was 56.47 MPa when the content of HAB reached 70 mol %. Failure morphologies confirmed that the interfacial adhesion of PI/EPs was enhanced owing to the surface activity of PI fibers. Consequently, this study provides an effective strategy to the long-standing problems of high mechanical performances and poor surface activity for traditional PI fibers used in the PFRPs industry.

Enhancing the Interfacial Shear Strength and Tensile Strength of Carbon Fibers through Chemical Grafting of Chitosan and Carbon Nanotubes.

Multi-scale "rigid-soft" material coating has been an effective strategy for enhancing the interfacial shear strength (IFSS) of carbon fibers (CFs), which is one of the key themes in composite research. In this study, a soft material, chitosan (CS), and a rigid material, carbon nanotubes (CNTs), were sequentially grafted onto the CFs surface by a two-step amination reaction. The construction of the "rigid-soft" structure significantly increased the roughness and activity of the CFs surface, which improved the mechanical interlocking and chemical bonding between the CFs and resin. The interfacial shear strength (IFSS) of the CS- and CNT-modified CFs composites increased by 186.9% to 123.65 MPa compared to the desized fibers. In addition, the tensile strength of the modified CFs was also enhanced by 26.79% after coating with CS and CNTs. This strategy of establishing a "rigid-soft" gradient modulus interfacial layer with simple and non-destructive operation provides a valuable reference for obtaining high-performance CFs composites.

Effect of the Chemical Properties of Silane Coupling Agents on Interfacial Bonding Strength with Thermoplastics in the Resizing of Recycled Carbon Fibers.

Upcycling recycled carbon fibers recovered from waste carbon composites can reduce the price of carbon fibers while improving disposal-related environmental problems. This study assessed and characterized recycled carbon fibers subjected to sizing treatment using N-(2-aminoethyl)-3-aminopropyltrimethoxysilane (APS) chemically coordinated with polyamide 6 (PA6) and polypropylene (PP) resins. Sizing treatment with 1 wt.% APS for 10 s yielded O=C-O on the surface of the carbon fiber, and the -SiOH in the APS underwent a dehydration-condensation reaction that converted O=C-O (lactone groups) into bonds of C-O (hydroxyl groups) and C=O (carbonyl groups). The effects of C-O and C=O on the interfacial bonding force increased to a maximum, resulting in an oxygen-to-carbon ratio (O/C) of 0.26. The polar/surface energy ratio showed the highest value of 32.29% at 10 s, and the interfacial bonding force showed the maximum value of 32 MPa at 10 s, which is about 15% better than that of commercial carbon fiber (PA6-based condition). In 10 s resizing treatments with 0.5 wt.% 3-methacryloxypropyltrimethoxysilane (MPS), C-O, C=O, and O=C-O underwent a dehydration-condensation reaction with -SiOH, which broke the bonds between carbon and oxygen and introduced a methacrylate group (H2C=C(CH3)CO2H), resulting in a significant increase in C-O and C=O, with an O/C of 0.51. The polar/surface free energy ratio was about 38% at 10 s, with the interfacial bonding force increasing to 27% compared to commercial carbon fiber (PP-based conditions). MPS exhibited a superior interfacial shear strength improvement, two times higher than that of APS, with excellent coordination with PP resin and commercial carbon fiber, although the interfacial bonding strength of the PP resin was significantly lower.

Interfacial Shear Strength of Single-Walled Carbon Nanotubes-Cement Composites from Molecular Dynamics and Finite Element Studies.

Carbon nanotubes (CNTs) are nanometer-sized structures that can be used to reinforce cement matrices. The extent to which the mechanical properties are improved depends on the interfacial characteristics of the resulting materials, that is, on the interactions established between the CNTs and the cement. The experimental characterization of these interfaces is still impeded by technical limitations. The use of simulation methods has a great potential to give information about systems lacking experimental information. In this work, molecular dynamics (MD) and molecular mechanics (MM) were used in conjunction with finite element simulations to study the interfacial shear strength (ISS) of a structure formed by a pristine single-walled CNT (SWCNT) inserted in a tobermorite crystal. The results show that, for a constant SWCNT length, ISS values increase when the SWCNT radius increases, while for a constant SWCNT radius, shorter lengths enhance ISS values.

Effect of different irrigating solutions and endodontic sealers on bond strength of the dentin-post interface with and without defects.

AIMS: To investigate how the interfacial shear strength of the dentin-post interface with and without defects changes for different combinations irrigant/sealer. METHODS: In forty human decoronated and instrumented teeth, fibreglass posts were inserted. The obtained root segments were randomly assigned to four different groups according to the irrigant adopted and the cement used to seal the root canal. The root segments were processed for metyl-methacrylate embedding. Serial sections were obtained and submitted to histomorphometric analyses in order to observe any defect of adhesion at the dentin-post interface and to measure the defects' dimension. The serial sections were also submitted to micro-push-out test. The measured shear strength values were subjected to statistical analysis by one-way ANOVA. The values of bond strength determined for the defective samples were correlated with the dimension of the defects. Finite element models were built to interpret and corroborate the experimental findings. RESULTS: ANOVA showed that the generic combination irrigant/sealer does not affect the interfacial shear strength values. The bond strength of the samples without defects was averagely twice as large as that of the defective samples. The defects occupying more than 12% of the total transverse section area of the endodontic cement layer led to a reduction of the bond strength of about 70%. The predictions of the finite element models were in agreement with the experimental results. CONCLUSION: Defects occupying less than 2% of the total transverse section area of the cement layer were shown to be acceptable as they have rather negligible effects on the shear strength values. Technologies/protocols should be developed to minimize the number and the size of the defects.

Towards Sustainable Composite Manufacturing with Recycled Carbon Fiber Reinforced Thermoplastic Composites.

Currently, the vast majority of composite waste is either landfilled or incinerated, causing a massive burden on the environment and resulting in the loss of potentially valuable raw material. Here, conventional pyrolysis and reactive pyrolysis were used to reclaim carbon fibers from aeronautical scrap material, and to evaluate the feasibility of using reclaimed carbon fibers in structural components for the automotive sector. The need for fiber sizing was investigated as well as the behavior of the fiber material in macroscopic impact testing. The fibers were characterized with the single fiber tensile test, scanning electron microscopy, and the microbond test. Critical fiber length was estimated in both polypropylene and polyamide matrices. Tensile strength of the fiber material was better preserved with the reactive pyrolysis compared to the conventional pyrolysis, but in both cases the interfacial shear strength was retained or even improved. The impact testing revealed that the components made of these fibers fulfilled all required deformation limits set for the components with virgin fibers. These results indicate that recycled carbon fibers can be a viable option even in structural components, resulting in lower production costs and greener composites.

Nanoindentation of Multifunctional Smart Composites.

Three multifunctional smart composites for next-generation applications have been studied differently through versatile nanoindentation investigation techniques. They are used in order to determine peculiarities and specific properties for the different composites and to study the charge/matrix, charge/surface, or smart functions interactions. At first, a mapping indentation test was used to check the distribution of hardness and modulus across a large region to examine any non-uniformity due to structural anomalies or changes in properties for a carbon nanotubes (CNTs)-reinforced polypropylene (PP V-2) nanocomposite. This smart composite is suitable to be used in axial impeller fans and the results can be used to improve the process of the composite produced by injection moulding. Secondly, the interfacial properties of the carbon fibre (CF) and the resin were evaluated by a push-out method utilizing the smaller indentation tip to target the individual CF and apply load to measure its displacement under loads. This is useful to evaluate the effectiveness of the surface modification on the CFs, such as sizing. Finally, nanoindentation at different temperatures was used for the probing of the in situ response of smart shape memory polymer composite (SMPC) usable in grabbing devices for aerospace applications. Furthermore, the triggering temperature of the shape memory polymer response can be determined by observing the change of indentations after the heating and cooling cycles.

Mechanical Properties of Cement Reinforced with Pristine and Functionalized Carbon Nanotubes: Simulation Studies.

Concrete is well known for its compression resistance, making it suitable for any kind of construction. Several research studies show that the addition of carbon nanostructures to concrete allows for construction materials with both a higher resistance and durability, while having less porosity. Among the mentioned nanostructures are carbon nanotubes (CNTs), which consist of long cylindrical molecules with a nanoscale diameter. In this work, molecular dynamics (MD) simulations have been carried out, to study the effect of pristine or carboxyl functionalized CNTs inserted into a tobermorite crystal on the mechanical properties (elastic modulus and interfacial shear strength) of the resulting composites. The results show that the addition of the nanostructure to the tobermorite crystal increases the elastic modulus and the interfacial shear strength, observing a positive relation between the mechanical properties and the atomic interactions established between the tobermorite crystal and the CNT surface. In addition, functionalized CNTs present enhanced mechanical properties.

One Surface Treatment, Multiple Possibilities: Broadening the Use-Potential of Para-Aramid Fibers with Mechanical Adhesion.

Aramid fibers are high-strength and high-modulus technical fibers used in protective clothing, such as bulletproof vests and helmets, as well as in industrial applications, such as tires and brake pads. However, their full potential is not currently utilized due to adhesion problems to matrix materials. In this paper, we study how the introduction of mechanical adhesion between aramid fibers and matrix material the affects adhesion properties of the fiber in both thermoplastic and thermoset matrix. A microwave-induced surface modification method is used to create nanostructures to the fiber surface and a high throughput microbond method is used to determine changes in interfacial shear strength with an epoxy (EP) and a polypropylene (PP) matrix. Additionally, Fourier transform infrared spectroscopy, atomic force microscopy, and scanning electron microscopy were used to evaluate the surface morphology of the fibers and differences in failure mechanism at the fiber-matrix interface. We were able to increase interfacial shear strength (IFSS) by 82 and 358%, in EP and PP matrix, respectively, due to increased surface roughness and mechanical adhesion. Also, aging studies were conducted to confirm that no changes in the adhesion properties would occur over time.

The Adhesion of Plasma Nanocoatings Controls the Shear Properties of GF/Polyester Composite.

High-performance fibre-reinforced polymer composites are important construction materials based not only on the specific properties of the reinforcing fibres and the flexible polymer matrix but also on the compatible properties of the composite interphase. First, oxygen-free (a-CSi:H) and oxygen-binding (a-CSiO:H) plasma nanocoatings of different mechanical and tribological properties were deposited on planar silicon dioxide substrates that closely mimic E-glass. The nanoscratch test was used to characterize the nanocoating adhesion expressed in terms of critical normal load and work of adhesion. Next, the same nanocoatings were deposited on E-glass fibres, which were used as reinforcements in the polyester composite to affect its interphase properties. The shear properties of the polymer composite were characterized by macro- and micromechanical tests, namely a short beam shear test to determine the short-beam strength and a single fibre push-out test to determine the interfacial shear strength. The results of the polymer composites showed a strong correlation between the short-beam strength and the interfacial shear strength, proving that both tests are sensitive to changes in fibre-matrix adhesion due to different surface modifications of glass fibres (GF). Finally, a strong correlation between the shear properties of the GF/polyester composite and the adhesion of the plasma nanocoating expressed through the work of adhesion was demonstrated. Thus, increasing the work of adhesion of plasma nanocoatings from 0.8 to 1.5 mJ·m-2 increased the short-beam strength from 23.1 to 45.2 MPa. The results confirmed that the work of adhesion is a more suitable parameter in characterising the level of nanocoating adhesion in comparison with the critical normal load.

Topography of the Interfacial Shear Strength and the Mean Intrinsic Tensile Strength of Hemp Fibers as a Reinforcement of Polypropylene.

The strength of the interphase between the reinforcements and the matrix has a major role in the mechanical properties of natural fiber reinforced polyolefin composites. The creation of strong interphases is hindered by the hydrophobic and hydrophilic natures of the matrix and the reinforcements, respectively. Adding coupling agents has been a common strategy to solve this problem. Nonetheless, a correct dosage of such coupling agents is important to, on the one hand guarantee strong interphases and high tensile strengths, and on the other hand ensure a full exploitation of the strengthening capabilities of the reinforcements. The paper proposes using topographic profile techniques to represent the effect of reinforcement and coupling agent contents of the strength of the interphase and the exploitation of the reinforcements. This representation allowed identifying the areas that are more or less sensitive to coupling agent content. The research also helped by finding that an excess of coupling agent had less impact than a lack of this component.

Effect of a Bio-Based Dispersing Aid (Einar® 101) on PLA-Arbocel® Biocomposites: Evaluation of the Interfacial Shear Stress on the Final Mechanical Properties.

In this paper, the production and the characterization of poly (lactic) acid (PLA)-based composites containing different amounts (from 10 wt.% to 25 wt.%) of ultra-short cellulose fibers (Arbocel 600 BE/PU) have been investigated. On the basis of a previous study, it was observed that the addition of the cellulose fibers led to an embrittlement of the composite. Consequently, in order to obtain a composite with enhanced impact resistance and elongation at break, the effect of the Einar 101 addition (a bio-based dispersing aid additive) was analyzed. The role of the adhesion between the fiber and the matrix, coupled with a better fiber dispersion, was thus evaluated. Also, the consequences on the final mechanical properties (tensile and impact test) caused by the Einar addition were investigated. Analytical models were also applied in order to obtain an evaluation of the variation of the interfacial shear stress (IFSS) (strictly correlated to the fiber-matrix adhesion) caused by the Einar introduction. Furthermore, due to the very low aspect ratio of the Arbocel fibers, a suitable Bader and Boyer model variation was adopted in order to have a better quantitative estimation of the IFSS value.

Evaluation of tissue ingrowth and reaction of a porous polyethylene block as an onlay bone graft in rabbit posterior mandible.

PURPOSE: A new form of porous polyethylene, characterized by higher porosity and pore interconnectivity, was developed for use as a tissue-integrated implant. This study evaluated the effectiveness of porous polyethylene blocks used as an onlay bone graft in rabbit mandible in terms of tissue reaction, bone ingrowth, fibrovascularization, and graft-bone interfacial integrity. METHODS: Twelve New Zealand white rabbits were randomized into 3 treatment groups according to the study period (4, 12, or 24 weeks). Cylindrical specimens measuring 5 mm in diameter and 4.5 mm in thickness were placed directly on the body of the mandible without bone bed decortication, fixed in place with a titanium screw, and covered with a collagen membrane. Histologic and histomorphometric analyses were done using hematoxylin and eosin-stained bone slices. Interfacial shear strength was tested to quantify graft-bone interfacial integrity. RESULTS: The porous polyethylene graft was observed to integrate with the mandibular bone and exhibited tissue-bridge connections. At all postoperative time points, it was noted that the host tissues had grown deep into the pores of the porous polyethylene in the direction from the interface to the center of the graft. Both fibrovascular tissue and bone were found within the pores, but most bone ingrowth was observed at the graft-mandibular bone interface. Bone ingrowth depth and interfacial shear strength were in the range of 2.76-3.89 mm and 1.11-1.43 MPa, respectively. No significant differences among post-implantation time points were found for tissue ingrowth percentage and interfacial shear strength (P>0.05). CONCLUSIONS: Within the limits of the study, the present study revealed that the new porous polyethylene did not provoke any adverse systemic reactions. The material promoted fibrovascularization and displayed osteoconductive and osteogenic properties within and outside the contact interface. Stable interfacial integration between the graft and bone also took place.

Cyclodextrin as sizing for carbon fibers: new bonding mechanism improves adhesion in carbon fiber reinforced epoxy resin.

In this study, ß-cyclodextrin was covalently bonded on carbon fibers and its influence through host-guest complex formation was analyzed. Since cyclodextrins act as host molecules for aromatic compounds, complex formations can be performed in carbon fiber reinforced epoxy resins, between the carbon fiber surface and the aromatic compounds of the surrounding plastic. This interface design leads to improved adhesion between fiber and plastic. An increase of the interfacial shear strength from 12 MPa to 38 MPa was detected. It was possible to increase the interfacial shear strength even further, to 41 MPa, through a prior complex formation with one of the plastics components. In addition to the micromechanical analysis, energy-dispersive x-ray spectroscopy and contact angle measurements were performed to confirm the covalent coating of cyclodextrin on the carbon fiber surface.