Tensile properties of Argiope trifasciata drag line silk obtained from the spider's web

The tensile properties of Argiope trifasciata (Argiopidae) drag line silk retrieved from mooring threads in the web were characterized. Scanning electron microscope images were used to determine the cross‐sectional area of the samples, allowing force‐displacement plots to be rescaled as stress–strain curves and to characterize fracture surfaces. Twenty‐eight samples were tested to obtain statistically significant values of the mechanical parameters (elastic modulus, stress and strain at the proportional limit, and tensile strength). The tensile strength of the material was subjected to a Weibull analysis—the first time that this has been attempted with a spider silk. A low value of the Weibull modulus, m = 3.4, was obtained, demonstrating that drag line monofilament does not have a sufficiently reliable tensile strength to function as an engineering material on its own. © 2001 John Wiley & Sons, Inc. J Appl Polym Sci 82: 2245–2251, 2001     

Mechanical properties of Bombyx mori silk yarns studied with tensile testing method

The mechanical properties of Bombyx mori silk yarns and baves were investigated with tensile testing method. After silk yarns were pre‐extended at different strain levels and fixed for a while followed by recovery process, the tensile characteristics were examined in detail. It was commonly observed that low preliminary extensions up to 2–3% do not cause the changes of the mechanical properties and stress‐strain curves because they result in small structural changes and distortions, which were recovered within relatively short time (～ 1 min) in recovery process. However, pre‐extension values >3% strain lead to great changes of the mechanical properties and fibre structure, i.e., the changes of the shape of stress‐strain curve where additional transition point was observed, increase in the rigidity and stress at rupture, but decrease in extensibility as a result of orientation and destruction of the fibre structure especially in the amorphous region. It was stated that silk fibre consists of two distinct deformation regions, namely first linear region extending up to 2–3% strain and the second region beyond 2–3% strain where the main reorganization processes of the fibre structure, that is, the straining of macromolecular chains especially in the amorphous regions, the orientation of structural units such as β‐sheet microcrystals in stretching direction, and the destruction of macromolecules take place. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2009     

Active control on molecular conformations and tensile properties of spider silk

The mechanical properties of spider dragline silk vary with the spinning conditions, and molecular conformation is one of the important factors for the strength and strain of materials. Four kinds of Araneus ventricosus spider dragline silk fibers, measured by Raman microscopic spectrometry, were produced under different conditions: (1) reeled at the rate of 2 cm/s; (2) secreted by a dropping spider from a 100‐cm‐high table; (3) spun by spiders raised in two different containers. The Raman spectra of these fibers showed that the spinning method and growing environment of spiders had evident influences on the molecular conformations and tensile properties of dragline silk, and the dragline silk obtained from a dropping spider contained the greatest number of molecules with highly oriented β‐sheet structures and gave higher stress/strain values. © 2004 Wiley Periodicals, Inc. J Appl Polym Sci 92: 901–905, 2004     

Tensile mechanical property evaluation of natural and epoxide-treated silk fibers

Silkworm cocoon silk and spider major ampullate (drag line) silk exhibit macroscopic tensile properties that, while impressive in the context of polymer fibers, are highly variable. The variability is linked to the cross-sectional geometry being nonuniform: silk fiber cross section changes significantly over distances that are small compared to the scale on which diameters are averaged by typical characterization techniques. This characteristic must be taken into account when evaluating chemical treatments (in the present case infiltrating with crosslinkable epoxide) that are aimed at improving strength or stiffness. The magnitude of any change in mechanical property must be considered in relation to the spread in values recorded prior to treatment. An apparent improvement in the mean value of a tensile property may turn out to be statistically insignificant when compared to the standard deviations associated with those data. Previous authors do not address this simple assessment of significance. © 1995 John Wiley & Sons, Inc.     

How Nanofibers Carry the Load: Toward a Universal and Reliable Approach for Tensile Testing of Polymeric Nanofibrous Membranes

Nanofibrous nonwovens show high versatility and outstanding properties, with reduced weight. Porous morphology, high material flexibility and deformability challenge their mechanical testing, severely affecting results reliability. Still today, a specific technical standard method to carry out tensile testing of nonwoven nanofibrous mats is lacking, as well as studies concerning tensile test data reliability. In this work, an accurate, systematic, and critical study is presented concerning tensile testing of nonwovens, using electrospun Nylon 66 random nanofibrous mats as a case study. Nanofibers diameter and specimen geometry are investigated to thoroughly describe the nanomat tensile behavior, also considering the polymer thermal properties, and the nanofibers crossings number as a function of the nanofibers diameter. Below a threshold value, which lies between 150 and 250 nm, the overall mat mechanical behavior changes from ductile to brittle, showing enhanced elastic modulus for a high number of nanofibers crossings. While specimen geometry does not affect tensile results. Stress–strain data are analyzed using a phenomenological data fitting model to better interpret the tensile behavior. The experimental results demonstrate the high reliability of the proposed mass-based load normalization, providing a simple, effective, and universally suitable method for obtaining high reproducible tensile stress–strain curves.     

Tensile testing and fracture mechanism analysis of polyvinyl alcohol nanofibrous webs

A tensile properties testing study was conducted to understand the influence of thickness, cross-head speed (speed of testing), gauge length (GL; specimen test length), and sample shape on important tensile properties of polyvinyl alcohol (PVA) nanofiber webs. The effects of each testing parameter on load at break, extension at break, Young's modulus, and tensile stress–strain curve of PVA nanofiber webs are analyzed. The Welch two sample t-tests show the significant difference among tested data. Using interaction plots, two-way analysis of variance, and margin mean plots, the interaction effects among testing parameters have been analyzed. Of all the factors, cross-head speed, the interaction among GL, and sample thickness (GL: Thickness) and the interaction among GL, testing speed and sample thickness (GL: Speed: Thickness) have significant influence on the tensile properties of PVA nanofiber webs. Moreover, the hypothesized model of mechanism of tensile strain–stress curve of PVA nanofiber webs has been proposed. Based on the model, the tensile strain–stress curve can be split into three stages: linear elastic, partial break up, and complete breakage. This study will provide a better understanding of tensile testing parameters' effects and their interaction effects on the tensile properties of nanowebs.     

Effect of degumming on the tensile properties of silkworm (Bombyx mori) silk fiber

Forcibly reeled silkworm (Bombyx mori) silk was used to study how exposure to a degumming treatment (boiling in distilled water for 30 min) affects tensile properties. Because forcibly reeled and naturally spun fibers exhibit comparable mechanical behavior, the results can be generalized to material obtained conventionally from cocoons. The effects of degumming include: a decrease in the initial elastic modulus, a decrease in the stress at the proportional limit (yield strength), a change in the qualitative shape of force‐displacement curves, and significant qualitative and quantitative variability in force‐displacement data from samples subjected to nominally identical degumming histories. Immersion in water at room temperature or heating in air at 100°C for 30 min are both qualitatively equivalent to a 30‐min degumming treatment in boiling water, in terms of the effect on silk tensile properties. © 2002 Wiley Periodicals, Inc. J Appl Polym Sci 84: 1431–1437, 2002; DOI 10.1002/app.10366     

Influence of morphology on rheological and mechanical properties of SEBS-toughened,glass-bead-filled isotactic polypropene

The influence of morphology of glass-bead-filled isotactic polypropene containing 0–20 vol% thermoplastic elastomers (TPE) on mechanical and rheological properties was investigated. Polystyrene-block-poly(ethene-co-but-1-ene)-block-polystyrene(SEBS) and the corresponding block copolymer grafted with maleic anhydrid (SEBS-g-MA) were used as thermoplastic elastomers, realizing, in the first case, a three-phase morphology with separately dispersed glass beads and SEBS particles. In the second case, SEBS-g-MA forms an elastomeric interlayer between glass beads and polypropene matrix, comprising core–shell particles. Young's modulus and tensile yield stress of the hybrid composites decrease with an increase in TPE volume fraction due to low stiffness and strength of TPE. In comparison with the three-phase morphology of hybrid composites with SEBS, SEBS-g-MA interlayers effect a reduced stiffness of the hybrid composites but improve interfacial adhesion and, thus, tensile yield stress. Rheological storage and loss moduli increase with an increase in glass bead and TPE volume fraction. Due to improved interfacial adhesion, melt elasticity and viscosity are enhanced by the SEBS-g-MA interlayer when compared with separately dispersed SEBS. Consequently, the reduced stiffening effect of the glass beads due to SEBS-g-MA interlayer decreases mechanical elasticity, whereas improved interfacial adhesion, also promoted by the SEBS-g-MA interlayer, enhances tensile yield stress and melt elasticity. © 1998 John Wiley & Sons, Inc. J Appl Polym Sci 69: 2499–2506, 1998     

Molecular order in spider major ampullate silk (dragline): Effects of spinning rate and post‐spin drawing

Optical birefringence measurements are used to characterize how the molecular order of spider (Nephila clavipes) major ampullate silk is affected by linear spinning rate, by the extent of post‐spin drawing, and by post‐spin drawing rate. Results are interpreted qualitatively in terms of a simple microstructural model, in which birefringence depends on both the overall degree of molecular orientation and the extent to which crystalline regions are present. In contrast to the behavior of conventional, synthetic polymers, birefringence is found to be an unreliable predictor of tensile stiffness: microstructural changes that lead to increased birefringence may leave stiffness unchanged or, in some cases, lower than before. It is unlikely that economic processing of silk‐like polymers into fiber that exhibits biomimetic tensile properties can be achieved with spinning followed by drawing, or with a single spinning step. Instead, spinning followed by thermochemical treatment under load may be needed to obtain the critical combination of molecular orientation and crystallinity in commercially satisfactory time scales. © 1999 John Wiley & Sons, Inc. J Appl Polym Sci 72: 895–903, 1999     

Study of the effect of poly(acrylonitrile‐co‐butadiene‐co‐styrene) on the mechanical properties of an epoxy system

The mechanical properties of an epoxy system containing a diglycidyl ether of bisphenol A and 1,3‐bis(aminomethylcyclohexane) modified with different amounts of poly(acrylonitrile‐co‐butadiene‐co‐styrene) (ABS) were studied. Properties examined include tensile stress, percentage strain, tensile modulus, and tensile toughness determined in tensile tests, Rockwell hardness, and energy and maximum force to break a specimen in Charpy impact tests. The effect of the modification produced with the ABS was also studied using statistical methods including analysis of variance and multiple comparisons. The obtained data showed a significant effect of the modification produced with the ABS on the mechanical properties of this epoxy system, especially with the amount of 5 ABS per hundred parts of resin on the tensile properties and on the hardness. © 2004 Wiley Periodicals, Inc. J Appl Polym Sci 92: 461–467, 2004     

Wet-spun conductive silk fibroin–polyaniline filaments prepared from a formic acid–shell solution

Shell wastes represent a considerable quantity of byproducts in the coastal area. From the viewpoint of ecofriendly and economical disposal, shell wastes are dissolved in formic acid to prepare an ionic liquid at room temperature and dissolve silk fibers to prepare a spinning solution. In this study, we developed conductive filaments made of silk fibroin (SF) and polyaniline (PANI) with wet-spinning techniques and a water coagulation bath. We then evaluated its surface morphologies and structural, mechanical, and electrical properties. The average diameters of the SF–PANI filaments increased with SF concentration from 8.0 to 14.0 wt % when PANI content was 0.1 wt %. The structure of SF–PANI filaments included the coexistence of silk I and silk II and was not affected by the addition of PANI. Moreover, the stress and strain of the SF–PANI filament were 4.46 ± 0.57 MPa and 16.18 ± 2.35%, respectively. After three drafts, the stress and strain of the SF–PANI filaments reached their maxima: 22.08 ± 0.2 MPa and 63.2 ± 2.56%, respectively. In addition, the electrical properties of the SF–PANI filaments increased with the addition of PANI. Thus, all data in this study suggest that recycled shell wastes can be reused as dissolution systems to prepare SF-based functional conductive filaments. © 2018 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2019 , 136, 47127.     

Deformation and energy-absorption characteristics of microcellular EPDM rubber

Compressive stress–strain properties of closed-cell microcellular EPDM rubber vulcanizates with and without a filler were studied with the variation of density. For filler variation studies, silica and carbon black (N330) were used. With a decrease in density, the stress–strain curve for microcellular EPDM behaves differently from that for the solid vulcanizates: The curve rises steeply when cell breakdown occurs. The compressive stress–strain properties are found to depend on the strain rate. The compression set at constant stress increases with decreasing density. The energy-absorption behavior was studied from the compressive stress–strain properties. The efficiency, E, and ideality, I, parameters were also determined as they are useful for the evaluation of closed-cell microcellular rubber as a cushioning and packaging material. These parameters were plotted against stress to find the maximum efficiency and maximum ideality region which will make these materials suitable for cushioning or packaging applications. © 1998 John Wiley & Sons, Inc. J Appl Polym Sci 68:263–269, 1998     

Recovery in spider silk fibers

The extreme toughness of spider silk is dependent on the silk's ability to dissipate most of the mechanical energy imparted to the fiber during loading processes through irreversible deformations. This basic property makes the tensile behavior of spider silk fibers depend on the silk's previous deformation history in a largely unpredictable way. The resulting variability often represents an insurmountable difficulty for both the characterization of the material and its practical usage. In this study, it was shown that spider silk is endowed with a property that allows to circumvent these problems: supercontraction, the large shrinkage of the longitudinal dimension of spider silk fibers in wet environments, recovers the tensile properties of deformed spider silk fibers in a repetitive and reproducible way. © 2004 Wiley Periodicals, Inc. J Appl Polym Sci 92: 3537–3541, 2004     

Tensile fatigue behavior of polyamide 66 nanofiber yarns

Nanofiber yarns with twisted and continuous structures have potential applications in fabrication of complicated structures such as surgical suture yarns, artificial blood vessels, and tissue scaffolds. The objective of this article is to characterize the tensile fatigue behavior of continuous Polyamide 66 (PA66) nanofiber yarns produced by electrospinning with three different twist levels. Morphology and tensile properties of yarns were obtained under static tensile loading and after fatigue loading. Results showed that tensile properties and yarn diameter were dependent on the twist level. Yarns had nonlinear time‐independent stress–strain behavior under the monotonic loading rates between 10 and 50 mm/min. Applying cyclic loading also positively affected the tensile properties of nanofiber yarns and changed their stress–strain behavior. Fatigue loading increased the crystallinity and alignment of nanofibers within the yarn structure, which could be interpreted as improved tensile strength and elastic modulus. POLYM. ENG. SCI., 55:1805–1811, 2015. © 2014 Society of Plastics Engineers     

Effect of the chain‐transfer‐agent content on the emulsion polymerization process and adhesive properties of poly(n‐butyl acrylate‐co‐acrylic acid) latexes

The effect of water on regenerated silkworm silk fibers has been studied and compared with that of water on natural silkworm silk fibers. Regenerated fibers are spun from an N‐methylmorpholine‐N‐oxide (NMMO) fibroin solution through a wet‐spinning process, leading to fibers with two distinct tensile behaviors, labeled as brittle and ductile, respectively. Regenerated fibers show a significant contraction when immersed in water. Contraction increases further after drying. In contrast, natural silkworm silk fibers show a negligible contraction when submerged in water. Regenerated fibers tested in water are considerably more compliant than samples tested in air, though their stiffness and tensile strength are significantly reduced. It has been shown that the tensile properties of brittle regenerated fibers can be modified by a wet‐stretching process, which consists of deforming the fiber while immersed in water. Regenerated wet‐stretched fibers always show a ductile behavior independent from their initial tensile behavior. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2008     

Preparation of electrospun silk fibroin nanofibers from solutions containing native silk fibrils

Electrospinning solutions containing native silk fibrils with varied diameter and length were firstly achieved by dissolving silk in CaCl₂/Formic acid solvents. The structure of nanofibrils significantly improved the spinnability of electrospinning solution. The diameter of electrospun silk fibroin (SF) nanofibers increased from 40 nm to 1.8 μm, which could be achieved through increasing the solution concentration from 2 to 10%, implying a good size control over a wide range in this process. The structure of SF nanofibers transferred from random coil to beta‐sheet, before and after ethanol treatment, respectively. The mechanical properties of the SF nanofibers were improved significantly with stress and strain at break of 11.15 MPa and 7.66% in dry state, and 3.32 MPa and 174.0% in wet state. The strategy for preparing SF nanofibers with improved mechanical properties and fiber diameter control over a wide range provides benefits for the application of this material. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 41236.     

Nonlinear stress properties of poly(styrene-block-butadiene-block-styrene) melt under elongational and shear deformation

Effects of block copolymerized structure on nonlinear stress properties under elongational and shear deformation were investigated. Samples used in this study were poly(styrene-block-butadiene-block-styrene) (SBS, weight rate of S/B = 40/60) and polystyrene (PS) as a reference. Tensile stress–strain and shear stress relaxation properties were measured at the molten state. SBS showed high elasticity after reaching the yield point under elongational deformation at room temperature. PS melt showed substantial tensile stress increase after the yield point as strain rates increased. However, SBS melt did not exhibit noticeable tensile stress rise at higher elongation, and this property was almost independent of strain rates. Stress relaxation experiments revealed that the damping function of SBS melt was more strain-softening than that of PS melt. The results suggested that the block copolymerized structure decreases melt elasticity under elongational and shear deformation. A transmission electron micrograph indicated that the lack of melt elasticity in SBS melt is caused by orientation of the lamellar structure toward the stretched direction during deformation. © 1995 John Wiley & Sons, Inc.     

The tensile behavior of off‐axis loaded plant fiber composites: An insight on the nonlinear stress–strain response

Composites in load‐bearing applications are often exposed to off‐axis loads. For plant fiber composites (PFCs) to be seriously and readily considered in structural applications, knowledge and reliable prediction of their response to off‐axis loads is critical. This article (i) characterizes the stress–strain response, (ii) investigates the tensile properties, and (iii) analyses the fracture modes, of unidirectional flax‐polyester composites subjected to off‐axis tensile loading. A key finding of this study is that due to the nonlinear stress–strain response of PFCs, the apparent stiffness of the composite reduces by ∼30% in the strain range of 0.05 to 0.25%. In addition, through cyclic tests on the composites, the elastic strain limit is found to be only ∼0.15%. This has major implications on the strain range to be used for the determination of the composite elastic Young's modulus. Consequently, it is proposed that the tensile modulus for PFCs should be measured in the strain range of 0.025 to 0.100%. Through comparison with experimental data, conventional composite micromechanical models are found to be adequate in quantitatively describing the tensile behavior of off‐axis loaded PFCs. The application of such models has also enabled the determination of, otherwise difficult to measure, material properties, such as fiber shear and transverse modulus. Off‐axis loaded PFCs fail by three distinct fracture modes in three different off‐axis ranges; each fracture mode produces a unique fracture surface. POLYM. COMPOS. 2012. © 2012 Society of Plastics Engineers     

The variability and interdependence of spider drag line tensile properties

There is considerable interest in producing fibres that mimic the impressive tensile properties of spider drag line silk. It must, however, be recognised that these properties have been assessed largely on the basis of their average values; there can be significant variability about these averages. The natural variability can also serve as a useful indicator of the range of values over which particular properties of biomimetic silk may be tailored. Here we quantify several tensile properties of drag line from Argiope trifasciata spiders. We distinguish between two groups of properties on the basis of their statistical coefficient of variation. There is significantly greater scope for tailoring the viscoplastic hardening aspects of drag line, compared to the variability of the initial elastic response or the yield strength. We also consider whether elastic modulus, yield strength and viscoplastic hardening can be controlled independently of one another.     

Rubber-toughened cycloolefin copolymers

The influence of polystyrene-block-poly(ethene-co-but-1-ene)-block-polystyrene (SEBS) on the mechanical properties of metallocene-based cycloolefin copolymers (COC) was studied. COC is an amorphous polymer with very high stiffness and yield stress, but poor impact strength. With increasing SEBS volume fraction the notched impact strength is increasing. Low-molecular-weight SEBS (M_w = 90 000 g mol^–1) is more effective as impact modifier than high-molecular-weight SEBS (M_w = 272 000 g mol^–1). This is due to smaller particle size obtained when dispersing low-molecular-weight SEBS. With reduced particle size the amount of particles and, consequently, the probability of initiation of micromechanical processes, such as crazes, is increasing. The stiffness and yield stress of COC are decreasing with increasing SEBS volume fraction, due to low stiffness and tensile strength of SEBS. Addition of ultrahigh-molecular-weight polyethene (UHMWPE) does not improve the stiffness/toughness balance.