Correlation between processing conditions, microstructure and mechanical behavior in regenerated silkworm silk fibers (original) (raw)

Study on the Mechanical Properties of Different Silkworm Silk Fibers

Journal of Composite Materials, 2009

Mechanical properties of Bombyx mori, twisted B. mori, and Tussah silk fibers were investigated. Their ultimate tensile strength, elongation at break, and Young’s modulus were examined by performing a uniaxial tensile test on a single fiber. Scanning electron microscopy was used to observe the morphology of two different types of silk fiber, and to measure their apparent diameters from which the cross-sectional area of the silk fiber for stress-strain analysis can be determined. Based on experimental results obtained, it was found that Tussah silk fiber has a relatively high extensibility as compared to B. mori silk fiber and other natural fibers. Weibull analysis was also used to quantify tensile strength reproducibility of the silk fiber. Both single and twisted B. mori silk fibers have a better reproducibility of tensile properties than Tussah silk fiber.

Mechanical properties and toughening mechanisms of natural silkworm silks and their composites

Journal of the Mechanical Behavior of Biomedical Materials, 2020

There is an emerging interest in natural silkworm silks as alternative reinforcement for engineering composites. Here, we summarize the research on two common silkworm silks and silk fibre reinforced plastics (SFRPs) from the authors over the past few years in the context of related research. Silk fibres from silkworms display good strength and toughness under ambient and cryogenic conditions owing to their elastic-plastic deformation mechanism. In particular, the wild Antheraea pernyi (A. pernyi) silk also displays micro-and nano-fibrillation as an important mechanism for toughness and impact resistance. For SFRP composites, we found: (i) it is critical to achieve silk fibre volume fraction to above 50% for an optimal reinforcement and toughening effect; (ii) the tougher A. pernyi silks present a better reinforcement and toughening agent than B. mori silks; (iii) impact and toughness properties are advantageous properties of SFRPs; (iv) hybridization of natural silk with other fibres can further improve the mechanical performance and economics of SFRPs for engineering applications; and (v) the lightweight structure designs can improve the service efficiency of SFRPs for energy absorption. The understanding on the comprehensive mechanical properties and the toughening mechanisms of silks and silk fibre-reinforced polymer composites (SFRPs) could provide key insights into material design and applications.

Origin of the variability of the mechanical properties of silk fibers: 4. Order/crystallinity along silkworm and spider fibers

Journal of Raman Spectroscopy, 2014

The comparison of the low wavenumber of polarized Raman spectra (50-300 cm -1 ) from Bombyx mori (fresh cocoons fibres, handstretched 'Crins de Florence' strings from the gland content, dried gland, regenerated silk films) and Nephila madagascarensis silks reveals the high polarisation of fibre modes and the absence of polarisation for dried gland and regenerated silk films. This is consistent with X-ray diffraction measurements. The orientation of the fibroin/spidroin chains is due to the stretching during production, as for advanced synthetic fibres. The bandwidth of the 'ordered chains' signature is almost the same for the different fibres. However, the degree of polarisation seems to be higher in the case of spider fibre. The huge bandwidth of low wavenumber components of regenerated films indicates high disorder. Measurements along the fibre point out conformation changes with a periodicity (~20 mm) related to the silkworm head motion during the fabrication of the cocoon.

Impact of physio-chemical spinning conditions on the mechanical properties of biomimetic spider silk fibers

Communications Materials

Artificial spider silk has emerged as a biobased fiber that could replace some petroleum-based materials that are on the market today. Recent progress made it possible to produce the recombinant spider silk protein NT2RepCT at levels that would make the commercialization of fibers spun from this protein economically feasible. However, for most applications, the mechanical properties of the artificial silk fibers need to be improved. This could potentially be achieved by redesigning the spidroin, and/or by changing spinning conditions. Here, we show that several spinning parameters have a significant impact on the fibers’ mechanical properties by tensile testing more than 1000 fibers produced under 92 different conditions. The most important factors that contribute to increasing the tensile strength are fast reeling speeds and/or employing post-spin stretching. Stretching in combination with optimized spinning conditions results in fibers with a strength of >250 MPa, which is the ...

Silk Fibers Extruded Artificially from Aqueous Solutions of Regenerated Bombyx mori Silk Fibroin are Tougher than their Natural Counterparts

Advanced Materials, 2009

The dragline silk of certain spiders has excellent tensile properties [1] that are maintained over a remarkable temperature range. Although the commercial Mulberry Silkworm (Bombyx mori) silk is considerably weaker and less tough than the best spider dragline silks, fibers with comprehensive mechanical properties approaching that of spiders can be obtained by force-reeling directly from silkworms. Remarkably, both spider and silkworm silks are spun naturally from aqueous protein solutions at very low hydraulic pressures and at ambient temperature, not requiring a noxious coagulation bath. These considerations have lead to the search for methods to extrude strong and tough fibers from regenerated silk protein solutions. The processes developed so far depend on extruding silk fibroin dissolved in formic acid, N-methyl morpholine N-oxide (NMMO), 1,1,1,3,3,3-hexafluoro-2-propanol (HFIP), [7] trifluoro-acetic acid (TFA), [5a] hexafluoroacetone (HFA) or 1-ethyl-3-methylimidazolium chloride, usually into a methanol bath. However, most of these silk solvents either severely degrade the silk fibroin or are too expensive or toxic for use in industrial processes. Moreover, in all cases described, fibers spun from silk fibroin generated fibers weaker than their natural counterparts, with the exception of Ha et al.'s use of fibroin dissolved in TFA. [5a] However, the cold methanol coagulation bath used in these examples produced fibers that were much larger than the natural ones, lacked smooth surfaces, and were so stiff in their as-extruded form that their tensile properties could only be brought above those of natural fibers by manual neck drawing. This, and the cost of TFA, render Ha et al.'s process [5a] unsuitable for industrial scale up.

Effect of water on Bombyx mori regenerated silk fibers and its application in modifying their mechanical properties

Journal of Applied …, 2008

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.

Development of a Process for the Spinning of Synthetic Spider Silk

ACS Biomaterials Science & Engineering, 2015

Spider silks have unique mechanical properties but current efforts to duplicate those properties with recombinant proteins have been unsuccessful. This study was designed to develop a single process to spin fibers with excellent and consistent mechanical properties. As-spun fibers produced were brittle, but by stretching the fibers the mechanical properties were greatly improved. A water-dip or water-stretch further increased the strength and elongation of the synthetic spider silk fibers. Given the promising results of the water stretch, a mechanical doublestretch system was developed. Both a methanol/water mixture and an isopropanol/water mixture were independently used to stretch the fibers with this system. It was found that the methanol mixture produced fibers with high tensile strength while the isopropanol mixture produced fibers with high elongation.

Relationship between microstructure and mechanical properties in spider silk fibers: identification of two regimes in the microstructural changes

Soft Matter, 2012

The relationship between microstructure and mechanical properties has been investigated in Argiope trifasciata dragline silk fibers (major ampullate silk, MAS) by X-ray diffraction, Raman spectroscopy and tensile testing. We have analyzed three fractions of the material, i.e. amorphous, highly oriented nanocrystals and weakly oriented material, for different values of the macroscopic alignment parameter a, calculated as the relative difference between the length of the fiber and its length when supercontracted. Two distinct regimes have been identified: for low values of the alignment parameter a, microstructural changes are dominated by the reorientation of the nanocrystals; however, at high values (a > 0.5) of the alignment parameter, an increase in the fraction of the crystalline phase is revealed. The two regimes are also reflected in the mechanical behaviour, which can be explained by microstructural changes. This finding of the two distinct regimes in the microstructural evolution, which separates the reorientation and the increase in the crystalline phase, will be valuable to develop and validate molecular models of natural and artificial silk fibers, as well as to deepen our present knowledge of the origin of the outstanding properties of MAS fibers. In addition, we have analyzed the characteristics of the crystal lattice, and discussed the relationship between the percentage of short sidechain residues and the unit cell dimensions in different silks.